WO2023221297A1 - 一种抗多发弹陶瓷的制备方法及防弹插板 - Google Patents

一种抗多发弹陶瓷的制备方法及防弹插板 Download PDF

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WO2023221297A1
WO2023221297A1 PCT/CN2022/109161 CN2022109161W WO2023221297A1 WO 2023221297 A1 WO2023221297 A1 WO 2023221297A1 CN 2022109161 W CN2022109161 W CN 2022109161W WO 2023221297 A1 WO2023221297 A1 WO 2023221297A1
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ceramic
bullet
aramid
sintering
insert plate
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PCT/CN2022/109161
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English (en)
French (fr)
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张虹
林文松
欧阳晓平
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浙江立泰复合材料股份有限公司
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    • 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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Definitions

  • the invention relates to a bulletproof insert plate material and a preparation method thereof, specifically a preparation method of multi-bullet resistant ceramics and a bulletproof insert plate.
  • Bulletproof ceramics are the core material of lightweight bulletproof inserts, which play a role in breaking bullets and dissipating energy against incoming bullets.
  • rapid-fire weapons has put forward a realistic demand for protective inserts to prevent multiple rounds.
  • the patent application number 201920946066.8 discloses a bulletproof insert plate structure, which is staggered and spliced by two layers of ceramic small plates to avoid the bulletproof weakness caused by the ceramic overlap seams and improve its ability to withstand multiple bullets.
  • the patent application number 201220010296.1 discloses a composite structure bulletproof material plate.
  • the core point is still a ceramic layer made of units composed of ceramic plates or ceramic particles.
  • the present invention provides a preparation method of multi-bullet resistant ceramics and a bulletproof insert plate, which solve the problems in the prior art. It is characterized by elastic ceramics made of silicon carbide, boron carbide or a combination of the two. After ultra-high temperature sintering, it has a coarse grain structure, higher and more uniform hardness and compressive strength, and has high impact resistance. brittleness.
  • the bulletproof insert plate made by combining this type of ceramics with an appropriate backing plate has low bulk density and high elastic resistance. It can be used as a human body protection insert plate to resist multiple rounds of small and medium-caliber bullets such as DBP95 type 5.8mm (steel core) bullets. Invasion.
  • the present invention provides a method for preparing multi-bullet-resistant ceramics, which involves sintering silicon carbide and/or boron carbide.
  • the sintering can be high-temperature sintering, reaction sintering, hot-pressing sintering or pressureless sintering.
  • reaction sintering has a sintering temperature of 1750°C to 1900°C and a holding time of 4 to 6 hours;
  • hot press sintering has a temperature of 2100°C to 2250°C and a pressure The temperature is 30MPa, and the holding time is 2 to 3 hours;
  • the pressureless sintering has a temperature of 2050°C to 2150°C, and a holding time of 3 to 5 hours.
  • the silicon carbide and/or boron carbide are obtained by ball milling and centrifugal atomization granulation with a molding agent or sintering aid, where the ball milling mixing time is 12-24 hours, and the inlet of centrifugal atomization granulation is The temperature is 150-210°C, and the outlet temperature is 80-110°C; the dosage of the molding agent or burning aid is 2%-15%.
  • the molding agent is one or more of phenolic resin, glucose, and epoxy resin
  • the burning aid is carbon (C), metal element (such as Al), metal oxide (such as Al 2 O 3 ), one or more types of borides (such as TiB 2 ), etc.
  • the ceramic has an average grain size of 200-380 ⁇ m, a Vickers hardness of 23.5GPa-34GPa, and a compressive strength of 2200MPa-3100MPa.
  • the invention provides an anti-multi-bullet ceramic protective insert plate based on the above-mentioned ceramic, wherein: a crack arresting layer, an anti-ballistic ceramic panel and The energy-absorbing back panel has an area density of less than 25kg/m 2 and can withstand penetration by four rounds of DBP95 5.8mm bullets. All back protrusions are less than 25mm.
  • the crack-stopping layer is composed of aramid woven fabric, with an area density of 0.4-0.8kg/m 2 ;
  • the areal density of the anti-ballistic ceramic panel is 10.5-13.5kg/m 2 ;
  • the energy-absorbing layer is thermally cured by laminating ultra-high molecular weight polyethylene woven fabrics with an area density of 9.2 to 14.0 kg/m 2 .
  • a support layer is also provided between the anti-ballistic ceramic panel and the energy-absorbing backboard.
  • the support layer is thermally cured by laminating carbon fiber non-woven fabrics or aramid non-woven fabrics, with an area density of 0 to 1.8 kg/ m2 .
  • the aramid woven fabric is para-aramid (aramid II) woven fabric or heterocyclic aramid (aramid III) woven fabric
  • the aramid weft-free fabric is para-aramid (aramid) Aromatic II) weftless fabric or heterocyclic aramid (aromatic III) weftless fabric.
  • the present invention provides a method for preparing the multi-bullet resistant ceramic protective insert plate, which includes the following steps:
  • the compounding conditions are 128°C, 25MPa, and the compounding time is 25-30 minutes. After compounding, it will be used as an energy-absorbing backboard;
  • the anti-cracking layer composed of aramid woven fabric, the anti-elastic ceramic panel obtained in step 1), and the energy-absorbing backing plate obtained in step 2) are laminated together through the adhesive layer in sequence, and are heated at 128°C and 1.0MPa pressure. Get compounded.
  • a support layer is also provided between the anti-ballistic ceramic panel and the energy-absorbing back panel, and the support layer (4) is made of aramid UD cloth.
  • the preparation step of the support layer is to press and compound aramid UD cloth.
  • the compounding conditions are 128°C, 25MPa, and the compounding time is 10 minutes.
  • the present invention adopts the strategy of high-strength, high-hardness and highly brittle anti-ballistic ceramics.
  • the ceramic fragments produced by the impact of each bullet with ceramics greatly consume the bullet's Due to the kinetic energy, the cracks produced by the ceramic plate near the impact point are widely spaced and have little impact on the anti-elastic properties of other impact points, thus improving the ability of the bulletproof insert plate to stably withstand multiple rounds.
  • the bulletproof insert plate composed of three or four layers of materials maintains the inherent advantages of light weight and high hardness of bulletproof ceramics.
  • the strong support of the ceramic back plate fully exerts the bullet-breaking performance of the ceramic; the ceramic bullet-facing surface
  • the anti-cracking layer effectively avoids secondary damage caused by the splashing of ceramic particles.
  • FIG. 1 is a schematic structural diagram of the bulletproof inserting plate of the present invention.
  • Figure 2 is a schematic diagram of the impact point position of the bulletproof insert plate
  • Figure 3 is an X-ray perspective photograph (top picture) and an appearance diagram (bottom picture) of the target plate corresponding to Example 1 after being hit by four rounds of DBP95 5.8mm (steel core) bullets. The picture shows the back);
  • Figure 4 is an X-ray perspective photograph (top picture) and an appearance diagram (bottom picture) of the target plate corresponding to Example 2 after being hit by four rounds of DBP95 5.8mm (steel core) bullets. The picture shows the back);
  • Figure 5 is an X-ray perspective photograph (top picture) and an appearance diagram (bottom picture) of the target plate corresponding to Example 3 after four rounds of DBP95 5.8mm (steel core) bullets were hit. The picture shows the back);
  • Figure 6 is an X-ray perspective photograph (top picture) and an appearance diagram (bottom picture) of the target plate corresponding to Example 4 after being hit by four rounds of DBP95 5.8mm (steel core) bullets.
  • the left picture shows the front, and the right picture shows the The picture shows the back);
  • Figure 7 shows the X-ray perspective photo (top photo) and the apparent morphology photo (bottom photo) of the target plate corresponding to Comparative Example 5 after being hit by four rounds of DBP95 5.8mm (steel core) bullets. The picture shows the back).
  • the bulletproof insert plate is composed of three layers of materials: a crack arresting layer, a ceramic panel, and an ultra-high molecular weight polyethylene energy-absorbing layer.
  • the ceramic panel material is silicon carbide and is manufactured by a reaction sintering process. Its specific preparation method is as follows:
  • Step 1) Mix silicon carbide powder and phenolic resin by ball milling (time: 15h), centrifugal atomization and granulation (inlet temperature 195°C, outlet temperature 90°C), in which the mass proportion of phenolic resin is 15%, and the mixed powder is pressed and formed. Finally, a silicon cake composed of metallic silicon powder as the main body is placed on the compact. In a vacuum environment, a silicon infiltration reaction is used to obtain a dense silicon carbide ceramic.
  • the reaction sintering temperature is 1800°C and the sintering holding time is 5 hours; the resulting carbonization
  • the main structural and performance indicators of silicon ceramics average grain size 210 ⁇ m, Vickers hardness (GB/T 16534-2009) 23.8GPa, compressive strength (GBT 4740-1999) 2250MPa, average fracture toughness (GB/T23806-2009) 1.75 MPa ⁇ m 1/2 ;
  • Step 2 Unfold and cut the ultra-high molecular weight polyethylene fiber (average molecular weight 3 million to 3.1 million) UD cloth, and place the cut ultra-high molecular weight polyethylene fiber UD cloth neatly on the mold of the heat press. Press and compound, the compounding conditions are 128°C, 25MPa, compounding time is 30 minutes, and it will be used as an energy-absorbing backing board after compounding.
  • Step 3) Aramid woven fabric (area density 0.4kg/m 2 , aramid woven fabric is para-aramid (aramid II) woven fabric or heterocyclic aramid (aramid III) woven fabric)
  • the crack arresting layer, the silicon carbide ceramic plate (area density 14.0kg/m 2 ) obtained in step 1), and the ultra-high molecular weight polyethylene fiber energy-absorbing backsheet (area density 10.2kg/m 2 ) obtained in step 2) are passed through EVA in sequence
  • the adhesive layers were laminated together and compounded under 128°C and 1.0MPa pressure to obtain a bulletproof insert with a size of 260mm ⁇ 325mm and an area density of 24.8kg/ m2 .
  • the thickness of each layer, overall thickness and specifications of the bulletproof insert are shown in Table 1. .
  • the above-mentioned bulletproof insert plates were tested in accordance with the "GA141-2010 police Body Armor" standard.
  • the appropriate parts of the upper left, lower right, lower left and upper right parts of the insert plates were used to defend against one DBP95 5.8mm (steel core) bullet.
  • Specific test conditions The distance between the impact point of the projectile and the edge of the insert plate is not less than 50mm, the distance between the two projectile impact points is 100 ⁇ 10mm, the bullet speed is 940 ⁇ 10m/s, the incident angle is 0°, and the shooting distance is 15m.
  • the bulletproof insert plate is composed of four layers of materials, including a crack arrester layer, a ceramic panel, an aramid fiber board, and an ultra-high molecular weight polyethylene energy-absorbing layer.
  • the ceramic panel material is boron carbide and is manufactured by a hot-pressing sintering process. Its specific preparation method is as follows:
  • Step 1) Mix boron carbide powder and phenolic resin by ball milling (time: 12h), centrifugal atomization and granulation (inlet temperature 180°C, outlet temperature 85°C). The mass proportion of phenolic resin is 2%. After the mixed powder is pressed and formed, In a vacuum environment, boron carbide ceramic panels were prepared by hot-pressing sintering. The hot-pressing sintering temperature was 2200°C, the pressure was 30MPa, and the holding time was 2 hours.
  • the main structural and performance indicators of the obtained boron carbide ceramics were: average grain size 350 ⁇ m, dimension Hardness (GB/T 16534-2009) 33.8GPa, compressive strength (GBT 4740-1999) 3050MPa, average fracture toughness (GB/T23806-2009) 1.25MPa ⁇ m 1/2 .
  • Step 2) Unfold and cut the aramid UD cloth and place it neatly on the mold of the hot press for pressing and compounding.
  • the compounding conditions are 128°C, 25MPa, and the compounding time is 10 minutes.
  • Step 3 Unfold and cut the ultra-high molecular weight polyethylene fiber (average molecular weight 3 million to 3.1 million) UD cloth, and place the cut ultra-high molecular weight polyethylene fiber UD cloth neatly on the mold of the heat press. Pressing and compounding, the compounding conditions are 128°C, 25MPa, and the compounding time is 25min.
  • Step 4) Combine the crack arresting layer composed of aramid woven fabric (area density 0.8kg/m 2 ), the boron carbide ceramic plate obtained in step 1) (area density 12.2kg/m 2 ), and the aramid fiber obtained in step 2)
  • the support layer (area density 1.8kg/m 2 ) and the energy-absorbing backboard (area density 9.8kg/m 2 ) composed of the ultra-high molecular weight polyethylene fiberboard obtained in step 3) are laminated together in sequence through an adhesive layer and heated at 128°C , compounded under a pressure of 1.0MPa to obtain a bulletproof insert plate with a size of 260mm ⁇ 325mm and an area density of 25kg/ m2 .
  • the above-mentioned bulletproof insert plates were tested in accordance with the "GA141-2010 police Body Armor" standard.
  • the appropriate parts of the upper left, lower right, lower left and upper right parts of the insert plates were used to defend against one DBP95 5.8mm (steel core) bullet.
  • Specific test conditions The distance between the impact point of the projectile and the edge of the insert plate is not less than 50mm, the distance between the two projectile impact points is 100 ⁇ 10mm, the bullet speed is 940 ⁇ 10m/s, the incident angle is 0°, and the shooting distance is 15m.
  • the bulletproof insert plate is composed of three layers of materials: a crack arresting layer, a ceramic panel, and an ultra-high molecular weight polyethylene energy-absorbing layer.
  • the ceramic panel material is boron carbide and is manufactured by a pressureless sintering process. Its specific preparation method is as follows:
  • the main structural performance indicators of the obtained boron carbide ceramic are: average grain size 300 ⁇ m, Vickers hardness (GB /T 16534-2009) 31.8GPa, compressive strength (GBT 4740-1999) 2950MPa, average fracture toughness (GB/T23806-2009) 1.75MPa ⁇ m 1/2 .
  • Step 2 Unfold and cut the ultra-high molecular weight polyethylene fiber (average molecular weight 3 million to 3.1 million) UD cloth, and place the cut ultra-high molecular weight polyethylene fiber UD cloth neatly on the mold of the heat press. Pressing and compounding, the compounding conditions are 128°C, 25MPa, and the compounding time is 25min.
  • Step 3) Combine the crack arresting layer composed of aramid woven fabric (area density 0.4kg/m 2 ), the boron carbide ceramic plate obtained in step 1) (area density 11.5kg/m 2 ), and the ultra-high Molecular weight polyethylene fiber energy-absorbing backsheets (area density 12.8kg/m 2 ) are laminated together through adhesive layers in sequence, and compounded under 128°C and 1.0MPa pressure to obtain a size of 260mm ⁇ 325mm and an area density of 24.9kg/m 2 bulletproof inserts.
  • the above-mentioned bulletproof insert plates were tested in accordance with the "GA141-2010 police Body Armor" standard.
  • the appropriate parts of the upper left, lower right, lower left and upper right parts of the insert plates were used to defend against one DBP95 5.8mm (steel core) bullet.
  • Specific test conditions The distance between the impact point of the projectile and the edge of the insert plate is not less than 50mm, the distance between the two projectile impact points is 100 ⁇ 10mm, the bullet speed is 940 ⁇ 10m/s, the incident angle is 0°, and the shooting distance is 15m.
  • the bulletproof insert plate is composed of three layers of materials: a crack arrester layer, a ceramic panel, and an ultra-high molecular weight polyethylene energy-absorbing layer.
  • the ceramic panel material is a complex ceramic composed of silicon carbide and boron carbide, which is made by reaction sintering. Craft manufacturing. Its specific preparation method is as follows:
  • Step 1) Mix boron carbide, silicon carbide powder and phenolic resin by ball milling (time: 20h), centrifugal atomization and granulation (inlet temperature 185°C, outlet temperature 90°C), where the mass ratio of boron carbide, silicon carbide, and phenolic resin is The ratio is 75:10:15.
  • a silicon cake composed of metallic silicon powder as the main body is placed on the compact. In a vacuum environment, the silicon infiltration reaction is used to obtain dense silicon carbide ceramics.
  • the reaction sintering temperature is 1820 °C, the sintering holding time is 5 hours; the main structural performance indicators of the obtained multi-phase ceramic: average grain size 250 ⁇ m, Vickers hardness (GB/T 16534-2009) 26.5GPa, compressive strength (GBT 4740-1999) 2710MPa, The average fracture toughness (GB/T23806-2009) is 1.85MPa ⁇ m 1/2 .
  • Step 2 Unfold and cut the ultra-high molecular weight polyethylene fiber (average molecular weight 3 million to 3.1 million) UD cloth, and place the cut ultra-high molecular weight polyethylene fiber UD cloth neatly on the mold of the heat press. Pressing and compounding, the compounding conditions are 128°C, 25MPa, and the compounding time is 25min.
  • Step 3) Combine the crack arresting layer composed of aramid woven fabric (area density 0.4kg/m 2 ), the composite ceramic panel obtained in step 1) (area density 14.2kg/m 2 ), and the ultra-high ceramic panel obtained in step 2) Molecular weight polyethylene fiber energy-absorbing backsheets (area density 10.2kg/m 2 ) are laminated together through adhesive layers in sequence, and compounded at 128°C and 1.0MPa pressure to obtain a size of 250mm ⁇ 300mm and an area density of 25.0kg/m 2 bulletproof inserts.
  • the above-mentioned bulletproof insert plates were tested in accordance with the "GA141-2010 police Body Armor" standard.
  • the appropriate parts of the upper left, lower right, lower left and upper right parts of the insert plates were used to defend against one DBP95 5.8mm (steel core) bullet.
  • Specific test conditions The distance between the impact point of the projectile and the edge of the insert plate is not less than 50mm, the distance between the two projectile impact points is 100 ⁇ 10mm, the bullet speed is 940 ⁇ 10m/s, the incident angle is 0°, and the shooting distance is 15m.
  • the bulletproof insert plate is composed of three layers of materials: a crack arresting layer, a ceramic panel, and an ultra-high molecular weight polyethylene energy-absorbing layer.
  • the ceramic panel material is silicon carbide and is manufactured by a reaction sintering process. Its specific preparation method is as follows:
  • Step 1) Mix silicon carbide powder and phenolic resin by ball milling (time: 15h), centrifugal atomization and granulation (inlet temperature 195°C, outlet temperature 90°C), in which the mass proportion of phenolic resin is 15%, and the mixed powder is pressed and formed. Finally, a silicon cake composed of metallic silicon powder as the main body is placed on the compact. In a vacuum environment, a silicon infiltration reaction is used to obtain a dense silicon carbide ceramic.
  • the reaction sintering temperature is 1630°C and the sintering holding time is 2 hours; the resulting carbonization
  • the main structural and performance indicators of silicon ceramics average grain size 54 ⁇ m, average Vickers hardness (GB/T 16534-2009) 22.0GPa, average compressive strength (GBT 4740-1999) 2110MPa, average fracture toughness (GB/T23806-2009 )2.75MPa ⁇ m 1/2 ;
  • Step 2 Unfold and cut the ultra-high molecular weight polyethylene fiber (average molecular weight 3 million to 3.1 million) UD cloth, and place the cut ultra-high molecular weight polyethylene fiber UD cloth neatly on the mold of the heat press. Press and compound, the compounding conditions are 128°C, 25MPa, and the compounding time is 30 minutes.
  • Step 3) Combine the crack arresting layer composed of aramid woven fabric (area density 0.4kg/m 2 ), the silicon carbide ceramic plate obtained in step 1) (area density 14.0kg/m 2 ), and the ultra-high Molecular weight polyethylene fiber energy-absorbing backsheets (area density 10.2kg/m 2 ) are laminated together through adhesive layers in sequence, and compounded at 128°C and 1.0MPa pressure to obtain a size of 260mm ⁇ 325mm and an area density of 24.8kg/m 2 bulletproof inserts.
  • aramid woven fabric area density 0.4kg/m 2
  • the silicon carbide ceramic plate obtained in step 1) area density 14.0kg/m 2
  • the ultra-high Molecular weight polyethylene fiber energy-absorbing backsheets area density 10.2kg/m 2
  • the above-mentioned bulletproof insert plates (six pieces) were tested in accordance with the "GA141-2010 Police Body Armor" standard.
  • the appropriate parts of the upper left, lower right, lower left and upper right parts of each insert plate were used to defend against one DBP95 type 5.8mm (steel core) ) bullet, specific test conditions: the distance between the impact point of the bullet and the edge of the insert plate is not less than 50mm, the distance between the two impact points is 100 ⁇ 10mm, the bullet speed is 940 ⁇ 10m/s, the incident angle is 0°, and the shooting distance is 15m.
  • the above-mentioned target test two of each of the six plates were penetrated by one shot.
  • the back convexity value of the unpenetrated impact point was 24.2 to 33.1mm, with an average of 27.9mm.
  • the bulletproof insert plate is composed of four layers of materials, including a crack arrester layer, a ceramic panel, an aramid fiber board, and an ultra-high molecular weight polyethylene energy-absorbing layer.
  • the ceramic panel material is boron carbide and is manufactured by a hot-pressing sintering process. Its specific preparation method is as follows:
  • Step 1) Mix boron carbide powder and molding agent by ball milling (time: 12h), centrifugal atomization and granulation (inlet temperature 185°C, outlet temperature 80°C). The mass proportion of molding agent is 2%. After the mixed powder is pressed and formed, In a vacuum environment, boron carbide ceramic panels were prepared by hot-pressing sintering. The hot-pressing sintering temperature was 1980°C, the pressure was 30MPa, and the holding time was 1 hour.
  • the main structural and performance indicators of the obtained boron carbide ceramics were: average grain size 50 ⁇ m, average Vickers hardness (GB/T 16534-2009) 32.0GPa, average compressive strength (GBT 4740-1999) 3010MPa, average fracture toughness (GB/T23806-2009) 3.25MPa ⁇ m 1/2 ;
  • Step 2) Unfold and cut the aramid UD cloth and place it neatly on the mold of the hot press for pressing and compounding.
  • the compounding conditions are 128°C, 25MPa, and the compounding time is 10 minutes.
  • Step 3 Unfold and cut the ultra-high molecular weight polyethylene fiber (average molecular weight 3 million to 3.1 million) UD cloth, and place the cut ultra-high molecular weight polyethylene fiber UD cloth neatly on the mold of the heat press. Pressing and compounding, the compounding conditions are 128°C, 25MPa, and the compounding time is 25min.
  • Step 4) Combine the crack arresting layer composed of aramid woven fabric (area density 0.8kg/m 2 ), the boron carbide ceramic plate obtained in step 1) (area density 12.2kg/m 2 ), and the aramid fiber obtained in step 2)
  • the support layer (area density 1.8kg/m 2 ) and the energy-absorbing backboard (area density 9.8kg/m 2 ) composed of the ultra-high molecular weight polyethylene fiberboard obtained in step 3) are laminated together in sequence through an adhesive layer and heated at 128°C , compounded under a pressure of 1.0MPa to obtain a bulletproof insert plate with a size of 260mm ⁇ 325mm and an area density of 25kg/ m2 .
  • the above-mentioned bulletproof insert plates (six pieces) were tested in accordance with the "GA141-2010 Police Body Armor" standard.
  • the appropriate parts of the upper left, lower right, lower left and upper right parts of each insert plate were used to defend against one DBP95 type 5.8mm (steel core) ) bullet, specific test conditions: the distance between the impact point of the bullet and the edge of the insert plate is not less than 50mm, the distance between the two impact points is 100 ⁇ 10mm, the bullet speed is 940 ⁇ 10m/s, the incident angle is 0°, and the shooting distance is 15m.
  • the distance between the impact point of the bullet and the edge of the insert plate is not less than 50mm
  • the distance between the two impact points is 100 ⁇ 10mm
  • the bullet speed is 940 ⁇ 10m/s
  • the incident angle is 0°
  • the shooting distance is 15m.
  • one of the six boards was penetrated by two shots, and one board was penetrated by one shot; the back convexity value of the unpenet
  • the bulletproof insert plate is composed of three layers of materials: a crack arresting layer, a ceramic panel, and an ultra-high molecular weight polyethylene energy-absorbing layer.
  • the ceramic panel material is boron carbide and is manufactured by a pressureless sintering process. Its specific preparation method is as follows:
  • Step 1) Ball mill and mix boron carbide powder and sintering aid powder (time: 16h), centrifugal atomization and granulation (inlet temperature 190°C, outlet temperature 95°C), where the sintering aid is a mixture of carbon and silicon carbide (1 : 2), the mass proportion of sintering aid is 12%, after the mixed powder is pressed and formed, it is sintered and kept at 1980°C for 2 hours;
  • the main structural performance indicators of the obtained boron carbide ceramic are: average grain size 35 ⁇ m, average Vickers hardness (GB /T 16534-2009) 29.5GPa, average compressive strength (GBT 4740-1999) 2900MPa, average fracture toughness (GB/T23806-2009) 3.05MPa ⁇ m 1/2 ;
  • Step 2 Unfold and cut the ultra-high molecular weight polyethylene fiber (average molecular weight 3 million to 3.1 million) UD cloth, and place the cut ultra-high molecular weight polyethylene fiber UD cloth neatly on the mold of the heat press. Pressing and compounding, the compounding conditions are 128°C, 25MPa, and the compounding time is 25min.
  • Step 3) Combine the crack arresting layer composed of aramid woven fabric (area density 0.4kg/m 2 ), the boron carbide ceramic plate obtained in step 1) (area density 11.5kg/m 2 ), and the ultra-high Molecular weight polyethylene fiber energy-absorbing backsheets (area density 12.8kg/m 2 ) are laminated together through adhesive layers in sequence, and compounded under 128°C and 1.0MPa pressure to obtain a size of 260mm ⁇ 325mm and an area density of 24.9kg/m 2 bulletproof inserts.
  • the above-mentioned bulletproof insert plates (six pieces) were tested in accordance with the "GA141-2010 Police Body Armor" standard. Each insert plate was used to defend against one DBP95 type 5.8mm (steel core) at the appropriate parts of the upper left, lower right, lower left and upper right parts of each insert plate. ) bullet, specific test conditions: the distance between the impact point of the bullet and the edge of the insert plate is not less than 50mm, the distance between the two impact points is 100 ⁇ 10mm, the bullet speed is 940 ⁇ 10m/s, the incident angle is 0°, and the shooting distance is 15m. In the above-mentioned target test, two of the six plates were penetrated by one shot each. The back convexity value of the unpenetrated impact point was 24.2 to 30.1mm, with an average of 27.0mm.
  • the bulletproof insert plate is composed of three layers of materials: a crack arrester layer, a ceramic panel, and an ultra-high molecular weight polyethylene energy-absorbing layer.
  • the ceramic panel material is a complex ceramic composed of silicon carbide and boron carbide, which is made by reaction sintering. Craft manufacturing. Its specific preparation method is as follows:
  • Step 1) Mix boron carbide, silicon carbide powder and phenolic resin by ball milling (time: 20h), centrifugal atomization and granulation (inlet temperature 185°C, outlet temperature 90°C), where the mass ratio of boron carbide, silicon carbide, and phenolic resin is The ratio is 75:10:15.
  • a silicon cake composed of metallic silicon powder as the main body is placed on the compact. In a vacuum environment, the silicon infiltration reaction is used to obtain dense silicon carbide ceramics.
  • the reaction sintering temperature is 1580 °C, the sintering holding time is 2 hours; the main structural performance indicators of the obtained multiphase ceramics: average grain size 45 ⁇ m, average Vickers hardness (GB/T16534-2009) 25.2GPa, average compressive strength (GBT 4740-1999) 2600MPa , average fracture toughness (GB/T23806-2009) 3.25MPa ⁇ m 1/2 .
  • Step 2 Unfold and cut the ultra-high molecular weight polyethylene fiber (average molecular weight 3 million to 3.1 million) UD cloth, and place the cut ultra-high molecular weight polyethylene fiber UD cloth neatly on the mold of the heat press. Pressing and compounding, the compounding conditions are 128°C, 25MPa, and the compounding time is 25min.
  • Step 3) Combine the crack arresting layer composed of aramid woven fabric (area density 0.4kg/m 2 ), the composite ceramic panel obtained in step 1) (area density 14.2kg/m 2 ), and the ultra-high ceramic panel obtained in step 2) Molecular weight polyethylene fiber energy-absorbing backsheets (area density 10.2kg/m 2 ) are laminated together through adhesive layers in sequence, and compounded at 128°C and 1.0MPa pressure to obtain a size of 250mm ⁇ 300mm and an area density of 25.0kg/m 2 bulletproof inserts.
  • the above-mentioned bulletproof insert plates (six pieces) were tested in accordance with the "GA141-2010 Police Body Armor" standard. Each insert plate was used to defend against one DBP95 type 5.8mm (steel core) at the appropriate parts of the upper left, lower right, lower left and upper right parts of each insert plate. ) bullet, specific test conditions: the distance between the impact point of the bullet and the edge of the insert plate is not less than 50mm, the distance between the two impact points is 100 ⁇ 10mm, the bullet speed is 940 ⁇ 10m/s, the incident angle is 0°, and the shooting distance is 15m. In the above-mentioned target test, three of the six boards were penetrated by one shot each. The back convexity value of the unpenetrated impact point was 24.2 to 29.1mm, with an average of 26.9mm.
  • the bulletproof insert plate is composed of four layers of materials, including a crack arrester layer, a ceramic panel, an aramid fiber board, and an ultra-high molecular weight polyethylene energy-absorbing layer.
  • the ceramic panel material is boron carbide and is manufactured by a hot-pressing sintering process. Its specific preparation method is as follows:
  • Step 1) Mix boron carbide powder and phenolic resin by ball milling (time: 12h), centrifugal atomization and granulation (inlet temperature 185°C, outlet temperature 80°C). The mass proportion of phenolic resin is 2%.
  • boron carbide ceramic panels were prepared by hot-pressing sintering. The hot-pressing sintering temperature was 2050°C, the pressure was 30MPa, and the holding time was 2 hours.
  • the main structural and performance indicators of the obtained boron carbide ceramics were: average grain size 63 ⁇ m, dimension Hardness (GB/T 16534-2009) 29.5GPa, compressive strength (GBT 4740-1999) 2600MPa;
  • Step 2) Unfold and cut the aramid UD cloth and place it neatly on the mold of the hot press for pressing and compounding.
  • the compounding conditions are 128°C, 25MPa, and the compounding time is 10 minutes.
  • Step 3 Unfold and cut the ultra-high molecular weight polyethylene fiber (average molecular weight 3 million to 3.1 million) UD cloth, and place the cut ultra-high molecular weight polyethylene fiber UD cloth neatly on the mold of the heat press. Pressing and compounding, the compounding conditions are 128°C, 25MPa, and the compounding time is 25min.
  • Step 4) Combine the crack arresting layer composed of aramid woven fabric (area density 0.8kg/m 2 ), the boron carbide ceramic plate obtained in step 1) (area density 12.2kg/m 2 ), and the aramid fiber obtained in step 2)
  • the support layer (area density 1.8kg/m 2 ) and the energy-absorbing backboard (area density 9.8kg/m 2 ) composed of the ultra-high molecular weight polyethylene fiberboard obtained in step 3) are laminated together in sequence through an adhesive layer and heated at 128°C , compounded under a pressure of 1.0MPa to obtain a bulletproof insert plate with a size of 260mm ⁇ 325mm and an area density of 25kg/ m2 .
  • the above-mentioned bulletproof insert plates were tested in accordance with the "GA141-2010 police Body Armor" standard.
  • the appropriate parts of the upper left, lower right, lower left and upper right parts of the insert plates were used to defend against one DBP95 5.8mm (steel core) bullet.
  • Specific test conditions The distance between the impact point of the projectile and the edge of the insert plate is not less than 50mm, the distance between the two projectile impact points is 100 ⁇ 10mm, the bullet speed is 940 ⁇ 10m/s, the incident angle is 0°, and the shooting distance is 15m.
  • Two identical target plates obtained by the above process were subjected to a target test.
  • the invention discloses a method for preparing a multi-bullet-resistant ceramic, especially a bullet-resistant ceramic composed of silicon carbide, boron carbide or a composite of the two. It is characterized in that the ceramic has a coarse grain structure after being sintered at ultra-high temperature. It has high and more uniform hardness and compressive strength, and has high impact brittleness. It is a ceramic with specific metallographic structure and mechanical properties.
  • the main mechanism of composite armor to resist bullet penetration is: the bullet-resistant ceramic panel uses its high hardness and high strength characteristics to exert bullet-breaking effect to fragment the invading bullet. In the process of continued penetration, the bullet interacts with the fragments generated by the ceramic fragmentation.
  • the counter-grinding further consumes the mass and kinetic energy of the bullet; the bullet after penetrating the ceramic panel causes the fiber material of the back plate to shear and elongate, thereby consuming the remaining kinetic energy of the bullet and trapping the bullet fragments in the back plate, thereby preventing the bullet from Penetrate armor.
  • the support material in the bulletproof back plate of the present invention has relatively high stiffness, which prevents the ceramic panel from excessive bending during bullet penetration and gives full play to the bullet-breaking effectiveness of the ceramic panel.
  • increasing the grain size of the ceramic microstructure can improve the hardness and compressive strength of the ceramic.
  • brittleness properties can also fully break the ceramic around the impact point, thereby increasing the consumption of the bullet's kinetic energy and mass, and also causing it to produce
  • the angle (spacing) between multiple cracks is larger, so that the subsequent impact point has a greater probability of being in a complete ceramic position, thus improving its ability to resist penetration.
  • the bulletproof insert plate made by combining this type of ceramics with an appropriate backing plate has low bulk density and high elastic resistance. It can be used as a human body protection insert plate to resist multiple rounds of small and medium-caliber bullets such as DBP95 type 5.8mm (steel core) bullets. Invasion.

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Abstract

本发明公开了一种抗多发弹陶瓷的制备方法及防弹插板，该陶瓷采用碳化硅和/或碳化硼烧结获得，所述烧结其为高温烧结、反应烧结、热压烧结或者无压烧结中的一种或几种，所述陶瓷的平均晶粒尺寸为200-380μm，维氏硬度为23.5GPa-34GPa，抗压强度为2200MPa-3100MPa；由表及里依次通过粘结剂粘结的止裂层(1)、抗弹陶瓷面板(2)和吸能背板(3)即得防弹插板，面密度小于25kg/m 2，可抵御四发DBP95式5.8mm弹侵彻不穿，所有背凸小于25mm，在保证防弹插板不被子弹击穿的前提下，有效降低了子弹侵彻时产生的背凸，充分满足新一代防护插板多方面的抗弹要求。

Description

一种抗多发弹陶瓷的制备方法及防弹插板 技术领域
本发明涉及的是一种防弹插板材料及其制备方法，具体是一种抗多发弹陶瓷的制备方法及防弹插板。
背景技术
抗弹陶瓷是轻质防弹插板的核心材料，对入侵的子弹起着破弹、耗能的作用。现代战场环境下，速射武器的广泛应用，对防护插板提出了防多发弹的现实需求。
申请号为202010643753.X的专利公开了一种紧密排列结构的抗弹陶瓷单元，通过小块陶瓷的拼接以提高大块装甲抗多发弹的能力。
申请号为201920946066.8的专利公开了一种防弹插板结构，通过两层陶瓷小板错层拼接以避免陶瓷搭接缝带来的抗弹弱点同时提高其抗多发弹的能力。
申请号为201220010296.1的专利公开了一种复合结构防弹材料板，其核心要点仍然是采用陶瓷板或陶瓷颗粒组成的单元拼接而成的陶瓷层。
采用小块陶瓷拼接方式可以在某种程度上降低着弹点附近陶瓷破碎对周边陶瓷单元的影响，使装甲的其它部分保持一定程度的完整性从而提高其抗多发弹的能力。但是，拼接缝隙带来的风险是显然易见的，而且拼接陶瓷板所带来的穿着舒适性较差，我国新版的《GA141-2010警用防弹衣》特别强调“用户在选择防弹衣时，应在符合标准的前提下充分考虑防弹衣的重量和舒适性，以提高防弹衣的穿着率。”目前，国内外主流的用户大多要求采用整板陶瓷作为防弹面板。
众多的研究文献在陶瓷中加入增韧相，希冀通过提高陶瓷韧性以提高陶瓷抗多发弹的能力。实测结果表明，在子弹高速冲击载荷作用下，常规的增韧措施并不能阻碍裂纹在陶瓷整板的扩展，对防弹插板抗多发弹的能力帮助有限。
发明内容
为了克服现有技术中存在的不足，本发明提供一种抗多发弹陶瓷的制备方法及防弹插板，解决了现有技术中存在的问题。其特征为碳化硅、碳化硼或者是两者复合而成的抗弹陶瓷，经过超高温度烧结后具有粗大的晶粒组织、更高更均匀的硬度和抗压强度、并具有较高的冲击脆性。将此类陶瓷与适当的背板复合而成的防弹插板，具有低容重、高抗弹性能，可作为人体防护插板，抵御DBP95式5.8mm(钢芯)弹等中小口径枪弹多发弹的侵袭。
为实现上述目的，本发明一种抗多发弹的陶瓷的制备方法，其为：将碳化硅和/或碳化硼烧结即可，所述烧结其为高温烧结、反应烧结、热压烧结或者无压烧结中的一种或 几种；其中，所述反应烧结，其烧结温度为1750℃～1900℃，保温时间在4～6小时；所述热压烧结，其温度为2100℃～2250℃，压力为30MPa，保温时间2～3小时；所述无压烧结，其温度在2050℃～2150℃，保温时间为3～5小时。
优选的，所述碳化硅和/或碳化硼，其为与成型剂或助烧剂进行球磨混合、离心雾化造粒获得，其中球磨混合的时间为12-24h，离心雾化造粒的进口温度150～210℃，出口温度80～110℃；所述成型剂或助烧剂的用量为2％-15％。
优选的，所述成型剂为酚醛树脂、葡萄糖、环氧树脂中的一种或几种，所述助烧剂为碳(C)、金属单质(如Al)、金属氧化物(如Al 2O 3)、硼化物(如TiB 2)等中的一种或几种。
优选的，所述陶瓷的平均晶粒尺寸为200-380μm，维氏硬度为23.5GPa-34GPa，抗压强度为2200MPa-3100MPa。
作为本发明的另一方面，本发明提供一种基于所述的陶瓷的抗多发弹陶瓷防护插板，其中：由表及里依次通过粘结剂粘结的止裂层、抗弹陶瓷面板和吸能背板，面密度小于25kg/m 2，可抵御四发DBP95式5.8mm弹侵彻不穿，所有背凸小于25mm。
优选的，所述止裂层由芳纶机织布组成，面密度为0.4～0.8kg/m 2；
所述抗弹陶瓷面板的面密度为10.5～13.5kg/m 2；
所述吸能层由超高分子量聚乙烯无纬布叠层热固化而成，面密度为9.2～14.0kg/m 2。
优选的，在抗弹陶瓷面板和吸能背板之间还设置支撑层，所述支撑层由碳纤维无纬布或芳纶无纬布叠层热固化而成，面密度为0～1.8kg/m 2。
优选的，所述的芳纶机织布为对位芳纶(芳Ⅱ)机织布或杂环芳纶(芳Ⅲ)机织布，所述的芳纶无纬布为对位芳纶(芳Ⅱ)无纬布或杂环芳纶(芳Ⅲ)无纬布。
作为本发明的另一方面，本发明提供一种所述的抗多发弹陶瓷防护插板的制备方法，其包括以下步骤，
1)用抗多发弹的陶瓷制备抗弹陶瓷面板
2)将超高分子量聚乙烯纤维UD布压制复合，复合条件为128℃，25MPa，复合时间25-30min，复合后即作为吸能背板；
3)将芳纶机织布组成的止裂层、步骤1)得到的抗弹陶瓷面板、步骤2)得到的吸能背板依次通过胶黏层叠合在一起，在128℃、1.0MPa压力下复合即得。
优选的，在抗弹陶瓷面板和吸能背板之间还设置支撑层，所述支撑层(4)由芳纶UD布制成。
优选的，所述支撑层的制备步骤为，将芳纶UD布压制复合，复合条件为128℃，25MPa，复合时间10min。
本发明具有以下有益效果：
1)针对小口径子弹的高速冲击对陶瓷面板的破碎状态，本发明采取高强高硬且高脆性抗弹陶瓷的策略，每发子弹与陶瓷撞击产生的陶瓷碎末极大程度地消耗了子弹的动能，陶瓷板在着弹点附近产生的裂纹间隔宽阔，对其它弹着点的抗弹性能影响小，从而提高了防弹插板稳定抗多发弹的能力。
2)三层或四层材料复合而成的防弹插板，保持了抗弹陶瓷固有的质量轻、硬度高的优点，陶瓷背板的强支撑充分发挥了陶瓷的破弹效能；陶瓷迎弹面的止裂层有效避免了陶瓷碎末飞溅造成的二次损伤。
3)高韧性高比吸能的吸能材料与支撑层背板的运用，在保证防弹插板不被子弹击穿的前提下，有效降低了子弹侵彻时产生的背凸，充分满足新一代防护插板多方面的抗弹要求。
附图说明
图1为本发明防弹插板的结构示意图；
图2为防弹插板弹着点位置示意图；
图3为实施例1对应的靶板在四发DBP95式5.8mm(钢芯)弹弹击后的X光透视照片(上图)和表观形貌图(下图，左图表示正面，右图表示背面)；
图4为实施例2对应的靶板在四发DBP95式5.8mm(钢芯)弹弹击后的X光透视照片(上图)和表观形貌图(下图，左图表示正面，右图表示背面)；
图5为实施例3对应的靶板在四发DBP95式5.8mm(钢芯)弹弹击后的X光透视照片(上图)和表观形貌图(下图，左图表示正面，右图表示背面)；
图6为实施例4对应的靶板在四发DBP95式5.8mm(钢芯)弹弹击后的X光透视照片(上图)和表观形貌图(下图，左图表示正面，右图表示背面)；
图7为对比例5对应的靶板在四发DBP95式5.8mm(钢芯)弹弹击后的X光透视照片(上图)和表观形貌图(下图，左图表示正面，右图表示背面)。
具体实施方式
下面将结合本发明实施例，对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
请参阅图1，防弹插板由止裂层、陶瓷面板、超高分子量聚乙烯吸能层等三层材料组成；所述陶瓷面板材料为碳化硅，由反应烧结工艺制造。其具体的制备方法如下：
步骤1)将碳化硅粉末与酚醛树脂球磨混合(时间：15h)、离心雾化造粒(进口温度195℃，出口温度90℃)，其中酚醛树脂的质量占比为15％，混合粉末压制成形后，压坯上放置由金属硅粉为主体组成的硅饼，在真空环境下，利用硅熔渗反应得到致密的碳 化硅陶瓷，反应烧结温度为1800℃，烧结保温时间为5小时；所得碳化硅陶瓷的主要组织性能指标：平均晶粒尺寸210μm，维氏硬度(GB/T 16534-2009)23.8GPa，抗压强度(GBT 4740-1999)2250MPa，平均断裂韧性(GB/T23806-2009)1.75MPa·m 1/2；
步骤2)将超高分子量聚乙烯纤维(平均分子量为300万～310万)UD布展开铺层裁切，将裁切的超高分子量聚乙烯纤维UD布整齐放在热压机的模具上进行压制复合，复合条件为128℃，25MPa，复合时间30min，复合后即作为吸能背板。
步骤3)将芳纶机织布(面密度0.4kg/m 2，芳纶机织布为对位芳纶(芳Ⅱ)机织布或杂环芳纶(芳Ⅲ)机织布)组成的止裂层、步骤1)得到的碳化硅陶瓷板(面密度14.0kg/m 2)、步骤2)得到的超高分子量聚乙烯纤维吸能背板(面密度10.2kg/m 2)依次通过EVA胶黏层叠合在一起，在128℃、1.0MPa压力下复合得到尺寸为260mm×325mm、面密度为24.8kg/m 2的防弹插板，防弹插板各层厚度、整体厚度和规格见表1。
按照《GA141-2010警用防弹衣》标准对上述防弹插板进行测试，在插板的左上、右下、左下、右上适当部位各防御一发DBP95式5.8mm(钢芯)弹，具体测试条件：弹着点距离插板边缘不小于50mm，两个弹着点之间距离100±10mm，子弹速度940±10m/s，入射角0°，射击距离15m。在上述靶试试验中，四发子弹都没有穿透，背凸数值为19.5～24.5mm，平均23.7mm。
实施例2
请参阅图1，防弹插板由止裂层、陶瓷面板、芳纶纤维板、超高分子量聚乙烯吸能层等四层材料组成；所述陶瓷面板材料为碳化硼，由热压烧结工艺制造。其具体的制备方法如下：
步骤1)将碳化硼粉末与酚醛树脂球磨混合(时间：12h)、离心雾化造粒(进口温度180℃，出口温度85℃)，酚醛树脂质量占比为2％，混合粉末压制成形后，在真空环境下，采用热压烧结制备碳化硼陶瓷面板，热压烧结温度为2200℃，压力为30MPa，保温时间为2小时；所得碳化硼陶瓷的主要组织性能指标：平均晶粒尺寸350μm，维氏硬度(GB/T 16534-2009)33.8GPa，抗压强度(GBT 4740-1999)3050MPa，平均断裂韧性(GB/T23806-2009)1.25MPa·m 1/2。
步骤2)将芳纶UD布展开铺层裁切后整齐放在热压机的模具上进行压制复合，复合条件为128℃，25MPa，复合时间10min。
步骤3)将超高分子量聚乙烯纤维(平均分子量为300万～310万)UD布展开铺层裁切，将裁切的超高分子量聚乙烯纤维UD布整齐放在热压机的模具上进行压制复合，复合条件为128℃，25MPa，复合时间25min。
步骤4)将芳纶机织布(面密度0.8kg/m 2)组成的止裂层、步骤1)得到的碳化硼陶瓷板(面密度12.2kg/m 2)、步骤2)得到的芳纶支撑层(面密度1.8kg/m 2)、步骤3)得到的超高分子量聚乙烯纤维板组成的吸能背板(面密度9.8kg/m 2)依次通过胶黏层叠合 在一起，在128℃、1.0MPa压力下复合得到尺寸为260mm×325mm、面密度为25kg/m 2的防弹插板。
按照《GA141-2010警用防弹衣》标准对上述防弹插板进行测试，在插板的左上、右下、左下、右上适当部位各防御一发DBP95式5.8mm(钢芯)弹，具体测试条件：弹着点距离插板边缘不小于50mm，两个弹着点之间距离100±10mm，子弹速度940±10m/s，入射角0°，射击距离15m。在上述靶试试验中，四发子弹都没有穿透，背凸数值为17.2～23.5mm，平均22.1mm。
实施例3
请参阅图1，防弹插板由止裂层、陶瓷面板、超高分子量聚乙烯吸能层等三层材料组成；所述陶瓷面板材料为碳化硼，由无压烧结工艺制造。其具体的制备方法如下：
步骤1)将碳化硼粉末与助烧剂粉末球磨混合(时间：16h)、离心雾化造粒(进口温度190℃，出口温度95℃)，其中，助烧剂为碳与碳化硅的混合物(1：2)，助烧剂质量占比为12％，混合粉末压制成形后，在2050℃烧结保温3小时；所得碳化硼陶瓷的主要组织性能指标：平均晶粒尺寸300μm，维氏硬度(GB/T 16534-2009)31.8GPa，抗压强度(GBT 4740-1999)2950MPa，平均断裂韧性(GB/T23806-2009)1.75MPa·m 1/2。
步骤2)将超高分子量聚乙烯纤维(平均分子量为300万～310万)UD布展开铺层裁切，将裁切的超高分子量聚乙烯纤维UD布整齐放在热压机的模具上进行压制复合，复合条件为128℃，25MPa，复合时间25min。
步骤3)将芳纶机织布(面密度0.4kg/m 2)组成的止裂层、步骤1)得到的碳化硼陶瓷板(面密度11.5kg/m 2)、步骤2)得到的超高分子量聚乙烯纤维吸能背板(面密度12.8kg/m 2)依次通过胶黏层叠合在一起，在128℃、1.0MPa压力下复合得到尺寸为260mm×325mm、面密度为24.9kg/m 2的防弹插板。
按照《GA141-2010警用防弹衣》标准对上述防弹插板进行测试，在插板的左上、右下、左下、右上适当部位各防御一发DBP95式5.8mm(钢芯)弹，具体测试条件：弹着点距离插板边缘不小于50mm，两个弹着点之间距离100±10mm，子弹速度940±10m/s，入射角0°，射击距离15m。在上述靶试试验中，四发子弹都没有穿透，背凸数值为19.2～24.6mm，平均23.2mm。
实施例4；
请参阅图1，防弹插板由止裂层、陶瓷面板、超高分子量聚乙烯吸能层等三层材料组成；所述陶瓷面板材料为碳化硅与碳化硼组成的复相陶瓷，由反应烧结工艺制造。其具体的制备方法如下：
步骤1)将碳化硼、碳化硅粉末与酚醛树脂球磨混合(时间：20h)、离心雾化造粒(进口温度185℃，出口温度90℃)，其中碳化硼、碳化硅、酚醛树脂的质量比为75:10:15，混合粉末压制成形后，压坯上放置由金属硅粉为主体组成的硅饼，在真空环境下，利用 硅熔渗反应得到致密的碳化硅陶瓷，反应烧结温度为1820℃，烧结保温时间为5小时；所得复相陶瓷的主要组织性能指标：平均晶粒尺寸250μm，维氏硬度(GB/T 16534-2009)26.5GPa，抗压强度(GBT 4740-1999)2710MPa，平均断裂韧性(GB/T23806-2009)1.85MPa·m 1/2。
步骤2)将超高分子量聚乙烯纤维(平均分子量为300万～310万)UD布展开铺层裁切，将裁切的超高分子量聚乙烯纤维UD布整齐放在热压机的模具上进行压制复合，复合条件为128℃，25MPa，复合时间25min。
步骤3)将芳纶机织布(面密度0.4kg/m 2)组成的止裂层、步骤1)得到的复相陶瓷面板(面密度14.2kg/m 2)、步骤2)得到的超高分子量聚乙烯纤维吸能背板(面密度10.2kg/m 2)依次通过胶黏层叠合在一起，在128℃、1.0MPa压力下复合得到尺寸为250mm×300mm、面密度为25.0kg/m 2的防弹插板。
按照《GA141-2010警用防弹衣》标准对上述防弹插板进行测试，在插板的左上、右下、左下、右上适当部位各防御一发DBP95式5.8mm(钢芯)弹，具体测试条件：弹着点距离插板边缘不小于50mm，两个弹着点之间距离100±10mm，子弹速度940±10m/s，入射角0°，射击距离15m。在上述靶试试验中，四发子弹都没有穿透，背凸数值为18.2～23.1mm，平均21.9mm。
对比例1：
除了碳化硅陶瓷的烧结温度和时间不同以外，其它工艺参数与实施例1相同。
请参阅图1，防弹插板由止裂层、陶瓷面板、超高分子量聚乙烯吸能层等三层材料组成；所述陶瓷面板材料为碳化硅，由反应烧结工艺制造。其具体的制备方法如下：
步骤1)将碳化硅粉末与酚醛树脂球磨混合(时间：15h)、离心雾化造粒(进口温度195℃，出口温度90℃)，其中酚醛树脂的质量占比为15％，混合粉末压制成形后，压坯上放置由金属硅粉为主体组成的硅饼，在真空环境下，利用硅熔渗反应得到致密的碳化硅陶瓷，反应烧结温度为1630℃，烧结保温时间为2小时；所得碳化硅陶瓷的主要组织性能指标：平均晶粒尺寸54μm，平均维氏硬度(GB/T 16534-2009)22.0GPa，平均抗压强度(GBT 4740-1999)2110MPa，平均断裂韧性(GB/T23806-2009)2.75MPa·m 1/2；
步骤2)将超高分子量聚乙烯纤维(平均分子量为300万～310万)UD布展开铺层裁切，将裁切的超高分子量聚乙烯纤维UD布整齐放在热压机的模具上进行压制复合，复合条件为128℃，25MPa，复合时间30min。
步骤3)将芳纶机织布(面密度0.4kg/m 2)组成的止裂层、步骤1)得到的碳化硅 陶瓷板(面密度14.0kg/m 2)、步骤2)得到的超高分子量聚乙烯纤维吸能背板(面密度10.2kg/m 2)依次通过胶黏层叠合在一起，在128℃、1.0MPa压力下复合得到尺寸为260mm×325mm、面密度为24.8kg/m 2的防弹插板。
按照《GA141-2010警用防弹衣》标准对上述防弹插板(六块)进行测试，在每块插板的左上、右下、左下、右上适当部位各防御一发DBP95式5.8mm(钢芯)弹，具体测试条件：弹着点距离插板边缘不小于50mm，两个弹着点之间距离100±10mm，子弹速度940±10m/s，入射角0°，射击距离15m。在上述靶试试验中，六块板各有两块板有一枪穿透，未穿透的着弹点的背凸数值为24.2～33.1mm，平均27.9mm。
对比例2：
除了碳化硼陶瓷的烧结温度和时间不同以外，其它工艺参数与实施例2相同。
请参阅图1，防弹插板由止裂层、陶瓷面板、芳纶纤维板、超高分子量聚乙烯吸能层等四层材料组成；所述陶瓷面板材料为碳化硼，由热压烧结工艺制造。其具体的制备方法如下：
步骤1)将碳化硼粉末与成型剂球磨混合(时间：12h)、离心雾化造粒(进口温度185℃，出口温度80℃)，成型剂质量占比为2％，混合粉末压制成形后，在真空环境下，采用热压烧结制备碳化硼陶瓷面板，热压烧结温度为1980℃，压力为30MPa，保温时间为1小时；所得碳化硼陶瓷的主要组织性能指标：平均晶粒尺寸50μm，平均维氏硬度(GB/T 16534-2009)32.0GPa，平均抗压强度(GBT 4740-1999)3010MPa，平均断裂韧性(GB/T23806-2009)3.25MPa·m 1/2；
步骤2)将芳纶UD布展开铺层裁切后整齐放在热压机的模具上进行压制复合，复合条件为128℃，25MPa，复合时间10min。
步骤3)将超高分子量聚乙烯纤维(平均分子量为300万～310万)UD布展开铺层裁切，将裁切的超高分子量聚乙烯纤维UD布整齐放在热压机的模具上进行压制复合，复合条件为128℃，25MPa，复合时间25min。
步骤4)将芳纶机织布(面密度0.8kg/m 2)组成的止裂层、步骤1)得到的碳化硼陶瓷板(面密度12.2kg/m 2)、步骤2)得到的芳纶支撑层(面密度1.8kg/m 2)、步骤3)得到的超高分子量聚乙烯纤维板组成的吸能背板(面密度9.8kg/m 2)依次通过胶黏层叠合在一起，在128℃、1.0MPa压力下复合得到尺寸为260mm×325mm、面密度为25kg/m 2的防弹插板。
按照《GA141-2010警用防弹衣》标准对上述防弹插板(六块)进行测试，在每块插板的左上、右下、左下、右上适当部位各防御一发DBP95式5.8mm(钢芯)弹，具体测试条件：弹着点距离插板边缘不小于50mm，两个弹着点之间距离100±10mm，子弹速度940±10m/s，入射角0°，射击距离15m。在上述靶试试验中，六块板有一块板有两枪穿透，有一块板有一枪穿透；未穿透的着弹点的背凸数值为19.2～28.5mm，平均25.5mm。
对比例3：
除了碳化硼陶瓷的烧结温度和时间不同以外，其它工艺参数与实施例3相同。
请参阅图1，防弹插板由止裂层、陶瓷面板、超高分子量聚乙烯吸能层等三层材料组成；所述陶瓷面板材料为碳化硼，由无压烧结工艺制造。其具体的制备方法如下：
步骤1)将碳化硼粉末与助烧结粉末球磨混合(时间：16h)、离心雾化造粒(进口温度190℃，出口温度95℃)，其中，助烧剂为碳与碳化硅的混合物(1：2)，助烧剂质量占比为12％，混合粉末压制成形后，在1980℃烧结保温2小时；所得碳化硼陶瓷的主要组织性能指标：平均晶粒尺寸35μm，平均维氏硬度(GB/T 16534-2009)29.5GPa，平均抗压强度(GBT 4740-1999)2900MPa，平均断裂韧性(GB/T23806-2009)3.05MPa·m 1/2；
步骤2)将超高分子量聚乙烯纤维(平均分子量为300万～310万)UD布展开铺层裁切，将裁切的超高分子量聚乙烯纤维UD布整齐放在热压机的模具上进行压制复合，复合条件为128℃，25MPa，复合时间25min。
步骤3)将芳纶机织布(面密度0.4kg/m 2)组成的止裂层、步骤1)得到的碳化硼陶瓷板(面密度11.5kg/m 2)、步骤2)得到的超高分子量聚乙烯纤维吸能背板(面密度12.8kg/m 2)依次通过胶黏层叠合在一起，在128℃、1.0MPa压力下复合得到尺寸为260mm×325mm、面密度为24.9kg/m 2的防弹插板。
按照《GA141-2010警用防弹衣》标准对上述防弹插板(六块)进行测试，在每一个插板的左上、右下、左下、右上适当部位各防御一发DBP95式5.8mm(钢芯)弹，具体测试条件：弹着点距离插板边缘不小于50mm，两个弹着点之间距离100±10mm，子弹速度940±10m/s，入射角0°，射击距离15m。在上述靶试试验中，六块板有两块板各有一枪穿透，未穿透的着弹点的背凸数值为24.2～30.1mm，平均27.0mm。
对比例4：
除了碳化硅/碳化硼复相陶瓷的烧结温度和时间不同以外，其它工艺参数与实施例4相同。
请参阅图1，防弹插板由止裂层、陶瓷面板、超高分子量聚乙烯吸能层等三层材料组成；所述陶瓷面板材料为碳化硅与碳化硼组成的复相陶瓷，由反应烧结工艺制造。其具体的制备方法如下：
步骤1)将碳化硼、碳化硅粉末与酚醛树脂球磨混合(时间：20h)、离心雾化造粒(进口温度185℃，出口温度90℃)，其中碳化硼、碳化硅、酚醛树脂的质量比为75:10:15，混合粉末压制成形后，压坯上放置由金属硅粉为主体组成的硅饼，在真空环境下，利用硅熔渗反应得到致密的碳化硅陶瓷，反应烧结温度为1580℃，烧结保温时间为2小时；所得复相陶瓷的主要组织性能指标：平均晶粒尺寸45μm，平均维氏硬度(GB/T16534-2009)25.2GPa，平均抗压强度(GBT 4740-1999)2600MPa，平均断裂韧性(GB/T23806-2009)3.25MPa·m 1/2。
步骤2)将超高分子量聚乙烯纤维(平均分子量为300万～310万)UD布展开铺层裁切，将裁切的超高分子量聚乙烯纤维UD布整齐放在热压机的模具上进行压制复合，复合条件为128℃，25MPa，复合时间25min。
步骤3)将芳纶机织布(面密度0.4kg/m 2)组成的止裂层、步骤1)得到的复相陶瓷面板(面密度14.2kg/m 2)、步骤2)得到的超高分子量聚乙烯纤维吸能背板(面密度10.2kg/m 2)依次通过胶黏层叠合在一起，在128℃、1.0MPa压力下复合得到尺寸为250mm×300mm、面密度为25.0kg/m 2的防弹插板。
按照《GA141-2010警用防弹衣》标准对上述防弹插板(六块)进行测试，在每一个插板的左上、右下、左下、右上适当部位各防御一发DBP95式5.8mm(钢芯)弹，具体测试条件：弹着点距离插板边缘不小于50mm，两个弹着点之间距离100±10mm，子弹速度940±10m/s，入射角0°，射击距离15m。在上述靶试试验中，六块板有三块板各有一枪穿透，未穿透的着弹点的背凸数值为24.2～29.1mm，平均26.9mm。
对比例5
基本工艺路线和装甲结构与实施例2类似。请参阅图1，防弹插板由止裂层、陶瓷面板、芳纶纤维板、超高分子量聚乙烯吸能层等四层材料组成；所述陶瓷面板材料为碳化硼，由热压烧结工艺制造。其具体的制备方法如下：
步骤1)将碳化硼粉末与酚醛树脂球磨混合(时间：12h)、离心雾化造粒(进口温度185℃，出口温度80℃)，酚醛树脂质量占比为2％，混合粉末压制成形后，在真空环境下，采用热压烧结制备碳化硼陶瓷面板，热压烧结温度为2050℃，压力为30MPa，保 温时间为2小时；所得碳化硼陶瓷的主要组织性能指标：平均晶粒尺寸63μm，维氏硬度(GB/T 16534-2009)29.5GPa，抗压强度(GBT 4740-1999)2600MPa；
步骤2)将芳纶UD布展开铺层裁切后整齐放在热压机的模具上进行压制复合，复合条件为128℃，25MPa，复合时间10min。
步骤3)将超高分子量聚乙烯纤维(平均分子量为300万～310万)UD布展开铺层裁切，将裁切的超高分子量聚乙烯纤维UD布整齐放在热压机的模具上进行压制复合，复合条件为128℃，25MPa，复合时间25min。
步骤4)将芳纶机织布(面密度0.8kg/m 2)组成的止裂层、步骤1)得到的碳化硼陶瓷板(面密度12.2kg/m 2)、步骤2)得到的芳纶支撑层(面密度1.8kg/m 2)、步骤3)得到的超高分子量聚乙烯纤维板组成的吸能背板(面密度9.8kg/m 2)依次通过胶黏层叠合在一起，在128℃、1.0MPa压力下复合得到尺寸为260mm×325mm、面密度为25kg/m 2的防弹插板。
按照《GA141-2010警用防弹衣》标准对上述防弹插板进行测试，在插板的左上、右下、左下、右上适当部位各防御一发DBP95式5.8mm(钢芯)弹，具体测试条件：弹着点距离插板边缘不小于50mm，两个弹着点之间距离100±10mm，子弹速度940±10m/s，入射角0°，射击距离15m。对上述工艺得到的两个完全相同的靶板进行靶试试验，其中一块靶板四发子弹没有穿透，背凸数值为24.2～32.5mm，平均28.9mm；另一个靶板第一、第二、第四发子弹未被击穿，第三发子弹被击穿。
归纳所有实施例及对比例的实施效果，如表1所示。
Figure PCTCN2022109161-appb-000001
Figure PCTCN2022109161-appb-000002
本发明公开一种抗多发弹陶瓷，尤其是碳化硅、碳化硼或者是两者复合而成的抗弹陶瓷的制备方法，其特征为陶瓷经过超高温度烧结后具有粗大的晶粒组织、更高更均匀的硬度和抗压强度、并具有较高的冲击脆性，是具有特定金相组织和力学性能的陶瓷。复合装甲抵御子弹侵彻的主要机理为：抗弹陶瓷面板利用其高硬度高强度的特性发挥破弹效能使入侵的子弹破碎，子弹在继续侵彻过程中与陶瓷碎裂产生的碎末产生强烈的对磨，进一步消耗子弹的质量和动能；穿透陶瓷面板后的子弹使背板纤维材料产生剪切和伸长，从而消耗子弹剩余的动能，并将子弹碎片陷入在背板中，从而防止子弹穿透装甲。本发明防弹背板中的支撑材料具有相对较高的刚度，防止陶瓷面板在子弹侵彻过程中产生过大的弯曲，充分发挥陶瓷面板的破弹效能。另外，提高陶瓷显微组织晶粒尺寸，可以提高陶瓷的硬度和抗压强度，适当的脆性性能还可以使弹着点周围的陶瓷充分破碎，从而增加对子弹动能和质量的消耗，也使其产生的多条裂纹之间的夹角(间距)更大，从而使后续的弹着点有更大的概率处于一个完整的陶瓷位置，从而提高其抵御侵彻的能力。将此类陶瓷与适当的背板复合而成的防弹插板，具有低容重、高抗弹性能，可作为人体防护插板，抵御DBP95式5.8mm(钢芯)弹等中小口径枪弹多发弹的侵袭。
另外，对于小口径的子弹，其在陶瓷面板产生的直接破碎范围(破碎锥面积)是较小的。但是，前一发子弹在陶瓷面板上产生的裂纹会直接影响后续弹着点的抗弹效能。理想状态是裂纹只限制于有限范围，但是，对于陶瓷这类脆性材料而言，这是不可能实 现的，这也是许多对陶瓷进行增韧的方案，实测效果不佳的主要原因。
以上所述仅是本发明的优选实施方式，应当指出：对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (10)

  1. 一种抗多发弹的陶瓷的制备方法，其特征在于：将碳化硅和/或碳化硼烧结即可，所述烧结其为高温烧结、反应烧结、热压烧结或者无压烧结中的一种或几种；
    其中，所述反应烧结，其烧结温度为1750℃～1950℃，保温时间在4～6小时；所述热压烧结，其温度为2100℃～2250℃，压力为30MPa，保温时间2～3小时；所述无压烧结，其温度在2000℃～2150℃，保温时间为3～5小时。
  2. 如权利要求1所述的抗多发弹的陶瓷的制备方法，其特征在于：所述碳化硅和/或碳化硼，其为与成型剂或助烧剂进行球磨混合、离心雾化造粒获得，其中球磨混合的时间为12-24h，离心雾化造粒的进口温度150～210℃，出口温度80～110℃；所述成型剂或助烧剂的用量为2％-15％。
  3. 权利要求1-2任一项所述的抗多发弹的陶瓷的制备方法获得的陶瓷，其特征在于：所述陶瓷的平均晶粒尺寸为200-380μm，维氏硬度为23.5GPa-34GPa，抗压强度为2200MPa-3100MPa。
  4. 基于权利要求3所述的陶瓷的抗多发弹陶瓷防护插板，其特征在于：由表及里依次通过粘结剂粘结的止裂层(1)、抗弹陶瓷面板(2)和吸能背板(3)，面密度小于25kg/m 2，可抵御四发DBP95式5.8mm弹侵彻不穿，所有背凸小于25mm。
  5. 如权利要求4所述的抗多发弹陶瓷防护插板，其特征在于：所述止裂层(1)由芳纶机织布组成，面密度为0.4～0.8kg/m 2；
    所述抗弹陶瓷面板(2)的面密度为10.5～14.5kg/m 2；
    所述吸能层由超高分子量聚乙烯无纬布叠层热固化而成，面密度为9.0～14.0kg/m 2。
  6. 如权利要求4或5所述的抗多发弹陶瓷防护插板，其特征在于：在抗弹陶瓷面板(2)和吸能背板(3)之间还设置支撑层(4)，所述支撑层(4)由碳纤维无纬布或芳纶无纬布叠层热固化而成，面密度小于1.8kg/m 2。
  7. 如权利要求6所述的抗多发弹陶瓷防护插板的制备方法，其特征在于：所述的芳纶机织布为对位芳纶(芳Ⅱ)机织布或杂环芳纶(芳Ⅲ)机织布，所述的芳纶无纬布为对位芳纶(芳Ⅱ)无纬布或杂环芳纶(芳Ⅲ)无纬布。
  8. 权利要求4-7所述的抗多发弹陶瓷防护插板的制备方法，其特征在于：包括以下步骤，
    1)用抗多发弹的陶瓷作为抗弹陶瓷面板(2)
    2)将超高分子量聚乙烯纤维UD布压制复合，复合条件为128℃，25MPa，复合时间25-30min，复合后即作为吸能背板(3)；
    3)将芳纶机织布组成的止裂层(1)、步骤1)得到的抗弹陶瓷面板(2)、步骤2)得到的吸能背板(3)依次通过胶黏层叠合在一起，在128℃、1.0MPa压力下复合即得。
  9. 如权利要求8所述的抗多发弹陶瓷防护插板的制备方法，其特征在于：在抗弹陶瓷面板(2)和吸能背板(3)之间还设置支撑层(4)，所述支撑层(4)由芳纶UD布制 成。
  10. 如权利要求9所述的抗多发弹陶瓷防护插板的制备方法，其特征在于：所述支撑层(4)的制备步骤为，将芳纶UD布压制复合，复合条件为128℃，25MPa，复合时间10min。
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