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CN115365504A - B 4 C/Al shell-like gradient armor and preparation method thereof - Google Patents

B 4 C/Al shell-like gradient armor and preparation method thereof Download PDF

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Publication number
CN115365504A
CN115365504A CN202211025773.6A CN202211025773A CN115365504A CN 115365504 A CN115365504 A CN 115365504A CN 202211025773 A CN202211025773 A CN 202211025773A CN 115365504 A CN115365504 A CN 115365504A
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shell
armor
gradient
sintering
preparation
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CN115365504B (en
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王东
刘庆
薛超
邱博
郁红陶
汪庆华
万宏强
韩权利
闫正虎
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Xian Technological University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
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    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B22F9/00—Making metallic powder or suspensions thereof
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    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
    • C22C29/062—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on B4C
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
    • C22C32/0057—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides based on B4C
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F41—WEAPONS
    • F41H—ARMOUR; ARMOURED TURRETS; ARMOURED OR ARMED VEHICLES; MEANS OF ATTACK OR DEFENCE, e.g. CAMOUFLAGE, IN GENERAL
    • F41H5/00—Armour; Armour plates
    • F41H5/02—Plate construction
    • F41H5/04—Plate construction composed of more than one layer
    • F41H5/0414—Layered armour containing ceramic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
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    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
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    • B22F9/00—Making metallic powder or suspensions thereof
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    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract

The invention relates toAn armor protective material, in particular to a material B 4 A C/Al shell-imitated gradient armor and a preparation method thereof. B is to be 4 C and Al powders as starting materials in accordance with B 4 The volume ratio of C is reduced from 100% to 0% to carry out proportioning, 3% of Ti powder of the initial raw material is added as an additive, B 4 When the content of C accounts for 100 percent, ti powder is not required to be added, and N fine mixed powder with different volume fractions are obtained by ultrasonic vibration stirring, ball milling mixing, drying, cooling and sieving; according to B 4 Sequentially loading the latter mixed powder into a graphite die from high C content to low C content, tabletting, and step-by-step multistage discharge plasma sintering to obtain B 4 The C/Al shell-like gradient armor. Preparation of the resulting B 4 The C/Al shell-like gradient armor has high density, uniform average grain size distribution of crystal grains, higher impact resistance and repeated hit resistance, and can be widely applied to individual protection, protection of important parts of military operation systems such as armored vehicles, aerospace, ships and the like.

Description

B 4 C/Al shell-like gradient armor and preparation method thereof
Technical Field
The invention relates to an armor protection material, in particular to a material B 4 A C/Al shell-imitated gradient armor and a preparation method thereof.
Background
With the rapid development of anti-armor weapons technology, the battlefield survivability of weaponry equipment puts higher requirements on the performance of armor protection materials, thereby promoting the greater development of armor protection materials. Armor protective materials are being developed toward strengthening, lightening, multi-functionalization and high efficiency. The ceramic material is toughened and widely applied to the field of military protection, and the performance difference of the double-laminated armor panel and the back plate widely used in the market at present is large, the interface impedance is not matched, and the anti-elasticity performance cannot be fully exerted. Compared with a ceramic/metal double-laminated armor, the gradient armor which simultaneously keeps high hardness and high strength of ceramic, high toughness of metal and high tensile strength has great improvement on the capabilities of energy absorption, fracture resistance and the like of the protective armor. In addition, the ceramic phase content of the gradient armor continuously changes along the thickness direction of the protective armor, the material performance also continuously changes along the thickness direction, and the interface strength is improved compared with that of a double-laminated armor. Finally, compared with the laminated composite material which still needs an adhesive process, the gradient composite material which allows direct sintering molding is relatively simple in process. The gradient composite material is an armor protection material with excellent performance, but because the gradient composite material applied to the field of armor in China is few, the performance data is incomplete, and the structure is single, the development of the gradient ceramic composite armor in China is greatly limited. Therefore, materials and structures are gradually becoming research hotspots in the field of developing novel gradient armor.
In the bullet-resistant ceramics, B 4 The C ceramic has the highest hardness and the lowest density, is the most ideal armor ceramic in terms of performance, and adopts B ceramic as the belly of the fuselage and the seats of passengers of the eagle armed helicopter in the United states 4 C and Kevlar. However, B is excellent in performance 4 The research on C ceramics currently stays in the field of double-laminated armor, and poor toughness always restricts B 4 C the main factor for ceramic applications, B 4 The C/Al composite material can improve the deficiency by compounding different volume fractions B 4 B formed of C/Al composite material 4 The C/Al gradient armor is one of the future development trends of the protective armor.
At present, B 4 The preparation of the C/Al composite material mostly adopts the traditional hot-pressing sintering technology, the sintering temperature for preparing the boron carbide ceramic is 2200 to 2300 ℃, and the heat preservation time is 0.5 to 2 hours. And (3) carrying out hot-pressing sintering for a long time at high temperature, so that the microstructure grains of the sample are coarse, and an impurity phase is generated at the grain boundary. In addition, when B is in the material 4 When the content of C exceeds 30%, under the action of long-time high-temperature sintering, metal aluminum with low melting point is inevitably precipitated, the material performance is reduced, even sintering preparation fails, and the defect also influences B 4 C/AAnd l, sintering preparation of the gradient armor.
According to the current research, 20vol.% B prepared at 1h and 620 ℃ is shown in Zhangpeng of Tai Yuan university 4 C/Al, hardness of only 1.09GPa. The high-content sodium carbonate is prepared into 40vol.% B by a vacuum hot pressing method under the sintering conditions that the sintering temperature and the heat preservation time are respectively 650 ℃ and 1h 4 C/Al, hardness of only 1.36GPa. It can be seen that the above researchers are preparing B because of the long-term high temperature sintering of hot-pressed vacuum sintering which degrades the material properties 4 The C/Al composite material is sintered at low temperature. However, due to the high melting point of the boron carbide particles, too low a sintering temperature does not guarantee the compactness of the composite material, along with B 4 Continuous increase of C particles, high content of B 4 B of C 4 The performance of the C/Al composite material is difficult to be exerted finally, so that the C/Al composite material has high content of B 4 C composite target board layer B 4 The C/Al gradient armor has the problems of low hardness of a target plate layer on the bullet-facing surface, poor shock resistance of the gradient armor, unsatisfactory repeated striking performance, low sintering preparation success rate and the like.
Disclosure of Invention
The invention aims at providing a compound B 4 A C/Al shell-like gradient armor and a preparation method thereof, aiming at overcoming the defect that the prior art has high content of B in the armor 4 B of C composite target plate layer 4 The sintering preparation problem of the C/Al gradient armor is solved, and the high content of B is effectively improved 4 B of C composite target plate layer 4 The hardness of the target plate layer of the bullet-facing surface of the C/Al gradient armor, the impact resistance of the gradient armor and the multiple-hit performance.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows: b 4 The preparation method of the C/Al shell-like gradient armor is characterized by comprising the following steps of:
the method comprises the following steps: b is to be 4 C and Al powders as starting materials in accordance with B 4 The volume ratio of C is reduced from 100% to 0% to carry out proportioning, 3% of Ti powder of the initial raw material is added as an additive, B 4 The content of C is 100 percent, ti powder is not added, and then B is respectively prepared 4 Suspensions of N grades with uniformly decreasing mass ratio of CCarrying out ultrasonic vibration stirring;
step two: pouring the mixed liquid into a ball milling tank, and carrying out ball milling for 12-15 h.
Step three: putting the slurry obtained by ball milling into a vacuum drying oven for drying for 3-5 h, cooling and sieving to obtain fine mixed powder of N different components;
step four: mixing B in 100% 4 C, putting the fine mixed powder into a graphite die, and tabletting to obtain a ceramic green body;
step five: carrying out plasma sintering on the formed ceramic green body to obtain B 4 Taking the 1 st layer of target plate material of the C/Al shell-imitated armor out of the mold, and grinding the surface graphite paper of the 1 st layer of target plate material;
step six: the layer 1 target plate material was reloaded into the graphite mold and the 2 nd species B obtained 4 The mixed powder with the C content reduced by one level is also put into a graphite die and is arranged above the layer 1 target plate material, and then the mixed powder is tabletted, molded and sintered by plasma again;
step seven: according to B 4 Sequentially filling the latter mixed powder into a graphite die from high to low in C content, taking the composite material in the overlapped area as a bonding layer according to the overlapped area existing in the sintering temperature interval of the composite material with different volume fractions, sintering other target plate materials with relatively low melting points on the basis of the overlapped area, and finally realizing the purpose that B is the target plate material with relatively low melting point 4 And sintering and preparing the C/Al shell-imitated gradient armor.
Further, in the first step, the suspension medium is absolute ethyl alcohol, and the ultrasonic vibration stirring time is 40-50 min.
Further, in the second step, absolute ethyl alcohol is selected as a ball milling medium, zirconia ceramics is selected as a milling ball, the ball-to-material ratio is set to be 8-10, and the ball milling rotating speed is 200r/min.
Further, in the third step, the drying temperature is set to be 140 ℃ in the vacuum drying oven.
Further, in the fifth step, the sintering parameters of the layer 1 target plate material are as follows: 30MPa, heating at 200 deg.C/min to 1200 deg.C, and sintering for 1min; after the temperature exceeds 1200 ℃, heating to 1700 ℃ at a speed of 100 ℃/min, and sintering for 11min in a heat preservation way; then cooling to 1000 ℃ at a speed of 100 ℃/min, and finally cooling to room temperature along with the furnace.
Further, in the sixth step, the sintering parameters of the 2 nd layer are as follows: 30MPa, heating at 200 deg.C/min to 1200 deg.C, and sintering at the same time for 1min; after the temperature is over 1200 ℃, heating to 1400 ℃ at a speed of 100 ℃/min, and sintering for 7min in a heat preservation way; then cooling to 1000 ℃ at a speed of 100 ℃/min, and finally cooling to room temperature along with the furnace.
Further, the fine mixed powder has a total of 6 grades, and the sintering parameters of the following 4 layers are as follows: 30MPa, the heat preservation time is respectively 7min, 11min, 7min and 7min, and the gradient is reduced by 200 ℃ from 1200 ℃.
Furthermore, before the last layer of tabletting is molded, the inner diameter of the graphite mold is phi 20mm, the diameter of the pressure head is phi 20mm, and the stress surface of the pressure head 1 is provided with a groove 2 in parallel.
Further, B prepared by the above preparation method 4 C/Al shell-like gradient armor.
Compared with the prior art, the invention has the following advantages:
1. b of the present invention 4 The C/Al shell-like gradient armor uses Al as a matrix phase and B 4 C is a reinforcing phase, and a small amount of Ti is added to improve the wettability between the matrix phase and the reinforcing phase. The structure between the target plate layers is improved through the grooving pressure head on the graphite die, the grooves with the depth of 1mm of the pressure head can form grooves on each layer of target plate material, so that each layer of target plate material is mutually occluded to form a mineral bridge interlocking structure, and sintering is carried out through a plasma sintering method, so that the prepared product has high density and uniform grain average particle size distribution.
2. B prepared in the invention 4 In the C/Al shell-like gradient armor, the material of the 1 st layer of target plate is B with the lowest density and the highest hardness in the bulletproof ceramic 4 C ceramic, which acts as an abrasive to bullets when resistant to penetration. Layer 2 target plate material (80 vol.% B) 4 C/Al composite) may be used as a bonding layer to bond B of the 1 st layer target plate material 4 C and layer 3 target plate material (60 vol.% B) 4 C/Al composite) is sintered into one body. In addition to this，80vol.％B 4 The C/Al composite material has higher hardness and certain toughness, and is used for the layer 1B 4 The C ceramic can play a strong supporting role. In the same way, the later layers of target plate materials are also used as bonding layers of the target material at the corresponding positions on the inner side.
3. The enrichment of the structure is an essential ring for the development of the gradient armor, and the structure of the natural biomaterial is imitated, so that the enrichment of the gradient ceramic composite armor structure is an effective and reasonable way. Of the many biomaterial structures, the natural ceramic with high strength and high toughness, shell, is the most valuable reference. The shell structure is composed of horny layer, prismatic layer and pearl layer, and the research of sufficient quantity shows that the mechanical property of high toughness of the shell mainly comes from the alternative lamination arrangement mode of pearl layer aragonite crystal and organic matrix. B of the present invention 4 The C/Al shell-like gradient armor interlayer structure is a mineral bridge interlocking structure of a shell-like pearl layer, crack expansion is hindered by the mineral bridge, crack deflection probability is increased, the mineral bridge is sheared and broken by pulling out the lamella, pulling-out resistance is further increased, toughness of the gradient armor is effectively enhanced, and penetration resistance is improved.
4. Compared with the traditional hot-pressing sintering technology, the discharge plasma sintering technology is characterized in that pulse current is directly introduced between powder particles under the pressurization condition to realize uniform heating sintering, and the multi-stage SPS discharge plasma sintering technology has the advantages of low sintering temperature and short heat preservation time in the plasma sintering technology, for example, in the preparation of B 4 When C is ceramic, the SPS discharge plasma sintering technology can reduce the sintering temperature to be within 1800 ℃, and the heat preservation time is at most 20min. The material prepared by sintering by adopting the method has more excellent performance and higher efficiency, and can realize the sintering preparation of the gradient armor. Especially when the sintering process difference between the target plate surface layer and the back layer is large, the step-by-step multi-section plasma sintering technology has important significance.
5. B prepared by the preparation process of the invention 4 The C/Al shell-like gradient armor material has higher impact resistance and repeated striking performance, and can be widely applied to individual protection,The protection of important parts of military operation systems such as armored vehicles, aerospace, ships and the like.
Drawings
FIG. 1 shows the different components B 4 And (5) fracture SEM of the C/Al composite material. (a) B is 4 C；(b)80vol.％B 4 C/Al；(c)60vol.％B 4 C/Al；(d)40vol.％B 4 C/Al；(e)20vol.％B 4 C/Al；(f)Al。
Figure 2 is a diagram of a grooving head on a graphite mold.
FIG. 3 is B 4 C/Al shell-like gradient armor sectional view.
Detailed Description
The present invention will be described in detail with reference to the following embodiments and drawings.
B according to the invention 4 The preparation method of the C/Al shell-like gradient armor adopts discharge plasma sintering to prepare a plurality of layers of different components B 4 The first attempt of C/Al composite material. The regulation and control of the ultrasonic vibration stirring process, the ball milling process, the sieving process and the plasma sintering process are B 4 The C/Al composite material has less pores and homogeneous average grain size distribution. The compact and uniform grain structure provides possibility for the excellence of the comprehensive mechanical property, and step-by-step multi-section sintering and the realization of a mineral bridge interlocking structure are not provided, so that the preparation method of the shell-like gradient armor with simplicity, high efficiency and high performance is obtained.
Example 1: b 4 The preparation method of the C/Al shell-like gradient armor specifically comprises the following steps:
the method comprises the following steps: the average particle diameter is 1 μm, the purity is 99%, B 4 Six grades of B with C contents of 100%, 80%, 60%, 40%, 20% and 0% respectively 4 C/Al composite material as initial material, ti powder in 3% of the initial material as additive, B 4 The Ti powder is not added in the initial raw materials with the C content accounting for 100 percent and 0 percent, the required mass is calculated according to the stoichiometric ratio, and then the raw materials are weighed. Preparing the weighed raw materials into suspension with the volume fraction of 2.0vol.% by taking absolute ethyl alcohol as a medium respectively, and stirring for 40min by ultrasonic vibration;
step two: pouring the suspension which is subjected to ultrasonic vibration and uniform stirring into a ball milling tank, adding a proper amount of zirconia balls, wherein the ball-material mass ratio is about 10;
step three: drying in ZK-40 type electric heating vacuum drying oven at 140 deg.C for 3 hr, cooling after vacuum drying, and sieving with 120 mesh sieve to obtain six kinds of uniform fine mixed powder;
step four: drying B 4 And C, filling the powder C into a graphite die with the inner diameter of phi 20mm, plugging the graphite die into a grooving pressure head on the graphite die, and compacting the graphite die on a tablet press under the pressure of 30MPa to prepare a cylindrical groove with the height of 2 mm.
Step five: putting the ceramic green body after tabletting forming and a graphite die into a plasma sintering furnace (30 MPa) together for sintering to obtain B 4 C, ceramic. In order to prevent the powder crystal grains from growing, the temperature is increased by 200 ℃/min before 1200 ℃; when the temperature reaches 1200 ℃, the mixture is sintered for 1min under the condition of heat preservation so as to eliminate gaps; after the temperature exceeds 1200 ℃, in order to obtain ceramics with excellent comprehensive performance, crystal grains need to be fully grown, so that the heating rate is reduced, the temperature is raised to 1700 ℃ at 100 ℃/min, and the temperature is kept for 11min; and finally cooling to 1000 ℃ at the speed of 100 ℃/min, then cooling to room temperature along with the furnace to obtain the shell-like gradient armor layer 1 target plate material, taking out the layer 1 target plate material from the mold, and grinding the surface graphite paper.
Step six: the obtained layer 1 target plate material was reloaded into a graphite mold and dried 80vol.% B 4 Loading C/Al powder into graphite mold, loading onto the layer 1 target plate, inserting into grooved pressure head of graphite mold, tabletting, and plasma sintering (30 MPa) to obtain B 4 The first 2 layers of target plate material of the C/Al imitation shell armor. In order to prevent the powder crystal grains from growing, the temperature is raised at 200 ℃/min before 1200 ℃; when the temperature reaches 1200 ℃, the mixture is sintered for 1min under the condition of heat preservation so as to eliminate gaps; after the temperature exceeds 1200 ℃, in order to obtain ceramics with excellent comprehensive performance, crystal grains need to be fully grown, so that the heating rate is reduced, the temperature is increased to 1400 ℃ at the speed of 100 ℃/min, and the temperature is kept for 7min; finally cooling to 1000 ℃ at a speed of 100 ℃/min, and then cooling to room temperature along with the furnaceAnd obtaining the front 2 layers of target plate materials of the shell-like gradient armor, taking out the front 2 layers of target plate materials from the die, and grinding the surface graphite paper of the target plate materials.
Step seven: the obtained first 2 layers of target plate material were reloaded into the graphite mold and dried 60vol.% B 4 Loading C/Al powder into graphite mold, placing above the front 2 layers of target plate material, plugging into grooved pressure head on the graphite mold, tabletting, and plasma sintering (30 MPa) to obtain B 4 The first 3 layers of target plate material of the C/Al shell-like armor. In order to prevent the powder crystal grains from growing, the temperature is raised at 200 ℃/min before 1000 ℃; when the temperature reaches 1000 ℃, the mixture is sintered for 1min under the condition of heat preservation so as to eliminate gaps; after the temperature exceeds 1000 ℃, in order to obtain ceramics with excellent comprehensive performance, crystal grains need to be fully grown, so that the heating rate is reduced, the temperature is increased to 1200 ℃ at the speed of 100 ℃/min, and the temperature is kept for 7min; and finally cooling to 1000 ℃ at a speed of 100 ℃/min, then cooling to room temperature along with the furnace to obtain the front 3 layers of target plate materials of the shell-like gradient armor, taking out the front 2 layers of target plate materials from the die, and grinding the surface graphite paper.
The first 3 layers of target plate material obtained were reloaded into a graphite mold and the dried 40vol.% B 4 Loading C/Al powder into graphite mold, loading onto the front 3 layers of target plate, inserting into grooved pressure head on the graphite mold, tabletting, and plasma sintering (30 MPa) to obtain B 4 The first 4 layers of target plate material of the C/Al imitation shell armor. In order to prevent the powder crystal grains from growing, the temperature is increased by 200 ℃/min before 800 ℃; when the temperature reaches 800 ℃, the mixture is sintered for 1min under the condition of heat preservation so as to eliminate gaps; after the temperature exceeds 800 ℃, in order to obtain ceramics with excellent comprehensive performance, crystal grains need to be fully grown, so that the heating rate is reduced, the temperature is raised to 1000 ℃ at the speed of 100 ℃/min, and the temperature is kept for 11min; and finally cooling to 800 ℃ at the speed of 100 ℃/min, then cooling to room temperature along with the furnace to obtain the front 4 layers of target plate materials of the shell-like gradient armor, taking out the front 4 layers of target plate materials from the die, and grinding the surface graphite paper.
The resulting first 4 layers of target plate material were reloaded into a graphite mold and dried 20vol.% B 4 Loading C/Al powder into graphite mold, loading onto the front 4 layers of target plate, inserting into grooved press head of graphite mold, and tablettingForm and plasma sintering (30 MPa) to obtain B 4 The first 5 layers of target plate material of the C/Al imitation shell armor. In order to prevent the powder crystal grains from growing, the temperature is raised at 200 ℃/min before 600 ℃; when the temperature reaches 600 ℃, the mixture is sintered for 1min in a heat preservation way to eliminate gaps; after the temperature exceeds 600 ℃, in order to obtain ceramics with excellent comprehensive performance, crystal grains need to be fully grown, so that the heating rate is reduced, the temperature is increased to 800 ℃ at the speed of 100 ℃/min, and the temperature is kept for 7min; and finally cooling to 600 ℃ at the speed of 100 ℃/min, then cooling to room temperature along with the furnace to obtain the front 5 layers of target plate materials of the shell-like gradient armor, taking out the front 5 layers of target plate materials from the die, and grinding the surface graphite paper.
The obtained front 5 layers of target plate materials are re-loaded into a graphite die, the dried Al powder is also loaded into the graphite die and is loaded above the front 5 layers of target plate materials, a normal pressure head is plugged in, tabletting forming is carried out again, and plasma sintering is carried out, thus obtaining B 4 C/Al shell-imitated armor. In order to prevent the powder crystal grains from growing, the temperature is increased by 20 ℃/min before 400 ℃; when the temperature reaches 400 ℃, the mixture is sintered for 1min under the condition of heat preservation so as to eliminate gaps; after the temperature exceeds 400 ℃, in order to obtain ceramics with excellent comprehensive performance, crystal grains need to be fully grown, so that the heating rate is reduced, the temperature is raised to 600 ℃ at the rate of 20 ℃/min, and the temperature is kept for 7min; and finally, cooling to 400 ℃ at the speed of 20 ℃/min, and then cooling to room temperature along with the furnace to obtain the shell-like gradient armor sample.
FIG. 1 shows Al,20vol.% B under Scanning Electron Microscopy (SEM) 4 C/Al、40vol.％B 4 C/Al、60vol.％B 4 C/Al、80vol.％B 4 C/Al、B 4 C, the cross section of the material is in micro-morphology. The pure Al bending fracture forms a relatively large area dimple after the tiny pores are gathered and interconnected in the plastic deformation process (see fig. 1 (a)), and the fracture form of the pure Al is relatively obvious ductile fracture. 20vol.% B compared to pure Al 4 The size of the dimple on the C/Al composite material section is reduced while the number of dimples is increased, besides, a plurality of fine B are arranged in and at the edge of the dimple 4 The C particles act to enhance the composite properties (see fig. 1 (b)). When B is present 4 B in C/Al composite material 4 When the C content reaches 40%, the size of the dimple on the cross section is reduced again, and the number of dimples is also reduced againIncrease, section B 4 C particles to 20vol.% B 4 C/Al is obviously increased, and the surface B of the composite material 4 C particles are uniformly distributed, but a small part of the agglomerated region still exists, and a small amount of pores exist in the agglomerated part (see fig. 1 (C)). When B is present 4 B in C/Al composite material 4 When the content of C reaches 60%, the dimple on the cross section is further reduced and is more evenly distributed on the agglomerated B 4 Around the C particles, numerous tiny pores are formed. The toughness of the material is reduced and the hardness is improved, but the overall properties of the material are slightly insufficient due to the presence of many pores (see fig. 1 (d)). With B 4 The content of C is increased to 80%, B 4 C appears in a more compact manner in a large area, and the dimples are almost invisible to be fused into the cross section, so that the number of pores is less, the toughness of the material is reduced, and the hardness is improved (see figure 1 (e)). Finally pure B 4 Micro-morphology of cross-section of C, B 4 The C ceramic is uniformly heated under pulse current and rapidly sintered, so as to avoid impurity phase (shown in figure 1 (f)) generated by coarse microstructure due to continuous high-temperature sintering, and B in the figure 4 The C ceramic is compact and has no obvious air holes.
The performance of the target plate material of the gradient armor is changed along with the change of the thickness, the preparation process is changed along with the change of the target plate material, and the mineral bridge interlocking structure of the shell-like gradient armor needs to be realized by the improved one-time SPS discharge plasma sintering method. The invention creatively adopts a multi-step and multi-section sintering method, firstly, the B with different components is prepared by sintering 4 And determining the optimal sintering temperature and the heat preservation time of the C/Al composite material. Then, the target plate material having a high melting point is sintered preferentially. And then according to the overlapping area existing in the sintering temperature interval of the composite materials with different volume fractions, taking the composite material in the overlapping area as a bonding layer, sintering other target plate materials with relatively low melting points on the basis of the bonding layer, and finally realizing the sintering preparation of the shell-like gradient armor.
Table 1 shows B in different volume fractions 4 The mechanical property of the C/Al composite material. From the table, follow B 4 Increase in volume fraction of C particles, B 4 The bending strength of the C/Al composite material as a whole also has an increasing tendency. Wherein, 60vol.% B 4 The bending resistance of C/Al is slightly reduced because of 1200 DEG CFail to make B 4 C is dense enough and high temperature makes the metal aluminum too active to form agglomerated B 4 C, the particle gaps flow out to form more air holes. B of different volume fractions 4 The hardness of the C/Al composite material follows that of B 4 The volume fraction of the C particles increases gradually, and the fracture toughness is opposite.
TABLE 1 different volume fractions of B 4 Mechanical property of the C/Al composite material.
Figure BDA0003815649020000091
Part B is prepared by vacuum hot-pressing sintering of doctor Chenhong Sheng of Taiyuan university 4 C/Al composite, B prepared therefrom, shown in Table 2 4 Mechanical property of the C/Al composite material.
TABLE 2 part of the preparation B by hot pressing sintering 4 The mechanical property of the C/Al composite material.
Figure BDA0003815649020000101
Comparing the mechanical properties shown in the two tables, the spark plasma sintering B adopted by the invention 4 Preparation of B by performance far-exceeding hot-pressing sintering of C/Al composite material 4 C/Al composite material, and to B 4 B with C content of more than 40% 4 And C/Al composite material is prepared. Research shows that B prepared by spark plasma sintering 4 The C/Al composite material can meet the performance requirement of each layer of target plate material of the shell-like gradient armor.
Referring to fig. 2, fig. 2 (b) is a top view of fig. 2 (a). The graphite mold comprises a pressure head 1, wherein grooves 2 are arranged on the stress surface of the pressure head 1 in parallel, the diameter of the pressure head is 20mm, the depth of each groove is 1mm, and the distance between every two grooves is 4mm.
Referring to fig. 3, it can be seen that the 1mm deep grooves of the custom indenter can form a groove in each layer of target plate material, allowing each layer of target plate material to interlock with each other to form a mineral bridge interlocking structure. The existence of the mineral bridge hinders crack propagation and increases crack deflection probability, and the mineral bridge is required to be sheared and broken by pulling out the lamella, so that the pulling-out resistance is further increased, and the toughness of the gradient armor is enhanced.
The invention is not limited to the embodiment examples, and any equivalent changes of the technical solution of the invention by the person skilled in the art after reading the description of the invention are covered by the claims of the present invention.

Claims (9)

1. B 4 The preparation method of the C/Al shell-like gradient armor is characterized by comprising the following steps of:
the method comprises the following steps: b is to be 4 C and Al powders as starting materials in accordance with B 4 The volume ratio of C is reduced from 100% to 0% to carry out proportioning, 3% of Ti powder of the initial raw material is added as an additive, B 4 The content of C is 100 percent, ti powder is not added, and then B is respectively prepared 4 Carrying out ultrasonic vibration stirring on the N grades of suspension liquid with the mass ratio of C being uniformly reduced;
step two: pouring the mixed liquid into a ball milling tank, and carrying out ball milling for 12-15 h.
Step three: putting the slurry obtained by ball milling into a vacuum drying oven for drying for 3-5 h, cooling and sieving to obtain fine mixed powder of N different components;
step four: mixing B in 100% 4 C, putting the fine mixed powder into a graphite die, and tabletting to obtain a ceramic green body;
step five: carrying out plasma sintering on the formed ceramic green body to obtain B 4 Taking the 1 st layer of target plate material of the C/Al shell-imitated armor out of the mold, and grinding the surface graphite paper of the 1 st layer of target plate material;
step six: the layer 1 target plate material was re-charged into a graphite mold, and the obtained species 2B was 4 The mixed powder with the C content reduced by one level is also put into a graphite die and is arranged above the layer 1 target plate material, and then the mixed powder is tabletted, molded and sintered by plasma again;
step seven: according to B 4 Sequentially filling the latter mixed powder with stone from high C content to low C contentAccording to the ink die, according to the overlapped area existing in the sintering temperature interval of the composite materials with different volume fractions, the composite materials in the overlapped area are used as the bonding layer, and other target plate materials with relatively low melting points are sintered on the basis of the overlapped area, so that the purpose of B 4 And (3) sintering and preparing the C/Al shell-like gradient armor.
2. A compound of claim 1 4 The preparation method of the C/Al shell-like gradient armor is characterized by comprising the following steps: in the first step, the medium of the suspension is absolute ethyl alcohol, and the ultrasonic vibration stirring time is 40-50 min.
3. A compound of claim 2 4 The preparation method of the C/Al shell-like gradient armor is characterized by comprising the following steps: in the second step, absolute ethyl alcohol is selected as a ball milling medium, zirconia ceramics is selected as a grinding ball, the ball-material ratio is set to be 8-10, and the ball milling rotating speed is 200r/min.
4. A B according to claim 3 4 The preparation method of the C/Al shell-like gradient armor is characterized by comprising the following steps: in the third step, the drying temperature is set to be 140 ℃ in a vacuum drying oven.
5. A B according to any one of claims 1-4 4 The preparation method of the C/Al shell-like gradient armor is characterized by comprising the following steps: in the fifth step, the sintering parameters of the layer 1 target plate material are as follows: 30MPa, heating at 200 deg.C/min to 1200 deg.C, and sintering for 1min; after the temperature exceeds 1200 ℃, heating to 1700 ℃ at a speed of 100 ℃/min, and sintering for 11min in a heat preservation way; then cooling to 1000 ℃ at a speed of 100 ℃/min, and finally cooling to room temperature along with the furnace.
6. A process according to claim 5 4 The preparation method of the C/Al shell-like gradient armor is characterized by comprising the following steps: in the sixth step, the sintering parameters of the 2 nd layer are as follows: 30MPa, heating at 200 deg.C/min to 1200 deg.C, and sintering for 1min; after the temperature exceeds 1200 ℃, the temperature is raised to 1400 ℃ at 100 ℃/minSintering at the temperature of 7min; then cooling to 1000 ℃ at a speed of 100 ℃/min, and finally cooling to room temperature along with the furnace.
7. A process according to claim 6 4 The preparation method of the C/Al shell-like gradient armor is characterized by comprising the following steps: the fine mixed powder has 6 grades, and the sintering parameters of the following 4 layers are as follows: 30MPa, the heat preservation time is respectively 7min, 11min, 7min and 7min, and the gradient is reduced by 200 ℃ from 1200 ℃.
8. A compound of claim 3 4 The preparation method of the C/Al shell-like gradient armor is characterized by comprising the following steps: before the last layer of tabletting is formed, the inner diameter of the graphite mould is phi 20mm, the diameter of the pressure head is phi 20mm, and the stress surface of the pressure head 1 is provided with a groove 2 in parallel.
9. A compound of claim 1 4 B prepared by C/Al shell-like gradient armor preparation method 4 The C/Al shell-like gradient armor.
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