A sheet-shaped TiB2 toughened B4C-SiC composite material and a preparation method thereof
By preparing sheet-like TiB2-toughened B4C-SiC composite materials through 3D printing and carbon-boron thermal reduction reaction, the problems of brittleness of B4C ceramics and density of SiC ceramics were solved, achieving composite ceramic armor with high fracture toughness and high strength, which is suitable for the field of ballistic armor.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-05-23
- Publication Date
- 2026-03-27
AI Technical Summary
Existing B4C ceramics are brittle and have low fracture toughness, making them difficult to form and sinter to achieve densification, which limits their application in bulletproof armor. SiC ceramics have a high density but high fracture toughness and impact resistance. TiB2 ceramics have high hardness and high toughness, but their high density makes it difficult to fabricate large-size and irregularly shaped structures.
Using filament extrusion 3D printing technology, composite filaments are prepared by thermoplastic polymer composite ceramic powder, and then sintered by carbon-boron thermal reduction reaction to generate sheet-like TiB2, which is uniformly distributed in B4C-SiC composite material to form a three-dimensional structure, thereby improving fracture toughness and strength.
The prepared sheet-like TiB2-toughened B4C-SiC composite material exhibits significantly improved fracture toughness and flexural strength, overcoming the difficulty of molding large-size and irregularly shaped structures using traditional methods, thus achieving high-performance composite ceramic armor.
Smart Images

Figure CN118324542B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The application provides a flaky TiB2 toughened B4C-SiC composite material and a preparation method thereof, and belongs to the field of ceramic materials. BACKGROUND
[0002] Bulletproof armor ceramics have the characteristics of high melting point, high hardness, high strength and low density, and are widely used in modern protection, national defense armored equipment such as human body, vehicle, helicopter, etc. The bulletproof ceramics used for protection armor currently include oxide ceramics represented by alumina and non-oxide ceramics represented by boron carbide, silicon carbide and titanium diboride. Among them, the anti-bullet performance of oxide ceramics is basically weaker than that of non-oxide ceramics. Among commonly used non-oxide ceramics, titanium diboride (TiB2) ceramic has the highest density and is mainly used for heavy armored vehicles; the density and hardness of silicon carbide ceramic are between those of boron carbide and alumina ceramic. It is worth noting that boron carbide ceramic (B4C) is the lightest bulletproof armor ceramic (2.52 g cm -3 ), in which the proportion of covalent bond between B and C is as high as 93% or more. The special bonding characteristics make it have high melting point (2450 °C), high modulus (450 GPa) and ultra-high hardness (> 30 GPa), and its hardness value is only lower than that of diamond and cubic boron nitride; at the same time, B4C has good chemical inertness, neutron absorption capacity (> 600 b) and thermoelectric performance. These excellent comprehensive properties make it popular in wear-resistant parts, ballistic armor, shielding materials, neutron absorbers and aerospace materials, etc.
[0003] At present, B4C has the following defects and prevents it from being widely used in bulletproof armor and other fields, mainly including the following points: on the one hand, it is brittle and has low fracture toughness (1.2-2.2 MPa·m 1 / 2 ), which makes it show the fatal defect of catastrophic failure and has poor use reliability; on the other hand, the ceramic has a high melting point and a low self-diffusion coefficient, which makes it difficult to be formed and sintered to be dense, which will limit the preparation of large-size and special-shaped structure B4C ceramics. At the same time, SiC ceramic has high hardness (~ 35 GPa), high melting point (~ 2700 °C), low density (3.2 g cm -3 ), high thermal conductivity (100-170 W·(m K) -1 ), high strength, corrosion resistance, wear resistance and excellent oxidation resistance, especially its high fracture toughness (~ 7.0 MPa·m 1 / 2 ) and impact resistance, therefore, SiC ceramic has broad application prospects as bulletproof armor ceramic. Compared with B4C ceramic, SiC ceramic has the advantages of low cost and high fracture toughness, but it has the disadvantage of large density.
[0004] In recent years, with the urgent demand and research and development of armored bulletproof protective equipment, ceramic composite armored bulletproof equipment has gradually replaced heavy homogeneous armor and become the direction of research and application in the field of armored protection. Titanium diboride (TiB2) ceramic is one of the most potential ceramics in armored bulletproof applications. The titanium atom layer is stacked in AAA order, and the six-coordinated boron atom is located at the center of the titanium atom triangular prism (H site), forming a strong covalent bonding hexagonal network structure. The overall stacking order is AHA-HAH… The Ti-B ionic bond between titanium atoms and boron atoms and the B-B covalent bond determine the high hardness (~30 GPa), high Young's modulus (~500 GPa), high strength (~460 MPa) and relatively high fracture toughness (~6.2 MPa·m 1 / 2 ) of TiB2 ceramic; at the same time, it has excellent thermodynamic stability, high melting point (3200 °C), high thermal conductivity (~100 W·(m K) -1 ), low thermal expansion coefficient (~4.6×10 −6 / ℃) and relatively high density (~4.53 g cm -3 ). Compared with B4C, SiC and TiB2 ceramics have higher Young's modulus and fracture toughness, which can effectively resist crushing and fracture during bulletproof process, but their density is larger. If SiC and TiB2 are introduced into B4C, not only can the rapid sintering densification be realized by adjusting the reaction sintering mechanism and microstructure, but also the fracture toughness of B4C can be improved and the composite ceramic armor can be lightened by preparing ternary composite structure, finally improving the armored bulletproof performance. Therefore, a preparation method of high-performance B4C-SiC / TiB2 composite bulletproof ceramic has become a research hotspot at home and abroad in recent years. At the same time, 3D printing technology for forming composite bulletproof ceramic has important significance for improving the structure size design and mechanical properties. SUMMARY
[0005] Therefore, the present application aims to provide a flaky TiB2 toughened B4C-SiC composite material and a preparation method thereof.
[0006] The present application is implemented by using the following technical solutions:
[0007] A flaky TiB2 toughened B4C-SiC composite material comprises ceramic aggregates and a binder; the ceramic aggregates are composed of SiB6, nano-carbon black and nano-flaky TiO2; and the binder is a mixture of ethylene-vinyl acetate copolymer and polyether sulfone resin.
[0008] The mass ratio of SiB6, nano-carbon black and nano-flaky TiO2 is 5-50:10-75:1-30.
[0009] The mass ratio of ethylene-vinyl acetate copolymer and polyether sulfone resin is 1:1-2.
[0010] The binder accounts for 10%-40% of the mass of the ceramic aggregates.
[0011] Preferably, the solvent is a mixture of N-methyl pyrrolidone and isopropyl alcohol.
[0012] More preferably, the volume ratio of N-methyl pyrrolidone and isopropyl alcohol in the solvent is 1-5:1.
[0013] The preparation method of the flaky TiB2 toughened B4C-SiC composite material comprises the following steps:
[0014] S1, weigh SiB6, carbon black and flaky TiO2 according to the proportion, mix them, and then put them in a solvent, mechanically stir them until they are uniform, and then deaerate to obtain a ceramic aggregate suspension, which is ready for use;
[0015] S2, adding ethylene-vinyl acetate copolymer and polyether sulfone in the ceramic aggregate suspension in proportion, ultrasonic dispersion treatment for 30-120 min, mechanical stirring for 24-60 h at a temperature of 50-80 DEG C, to obtain ceramic slurry;
[0016] S3, using a syringe pump to vertically inject the ceramic slurry into water, standing for 6-12 h for liquid-solid phase conversion, then filtering and naturally drying to obtain ceramic filaments, ready for use;
[0017] S4, melt extrusion 3D printing of the ceramic filaments, cooling after printing to obtain a printing blank;
[0018] S5, carbonization pyrolysis of the printing blank after heating to 800-1400 DEG C, wherein the pyrolysis atmosphere is a mixture of hydrogen and argon, and the SiB6-C-TiO2 composite material blank is obtained after pyrolysis;
[0019] S6, heating the SiB6-C-TiO2 composite material blank to 1600-2000 DEG C under inert atmosphere protection, holding sintering for 1-6 h, and cooling after sintering to obtain a sheet-shaped TiB2 toughened B4C-SiC composite material.
[0020] Preferably, the ultrasonic power in step S2 is 300-1000 W, and the mechanical stirring speed is 300-600 r / min.
[0021] Preferably, the injection rate in step S3 is 2.5-8.0 mL / min, and the syringe needle hole diameter is 2-8 mm.
[0022] Preferably, the heating temperature in step S4 melt extrusion 3D printing is 200-400 DEG C, and the printing speed is 4.0-20 mm / s.
[0023] Preferably, the volume ratio of hydrogen to argon in step S5 is 1:9, the heating rate is 5-10 DEG C / min, and the carbonization pyrolysis time is 2-8 h.
[0024] Preferably, the inert atmosphere in step S6 is argon.
[0025] Preferably, the heating and cooling rates in step S6 are both 20-100 DEG C / min.
[0026] Compared with the prior art, the present application has the following advantages:
[0027] (1) The application adopts reaction pressureless sintering auxiliary fuse extrusion type 3D printing technology to prepare flaky TiB2 toughened B4C-SiC three-dimensional structure composite material.
[0028] (2) The application uses flaky TiO2 as a template agent and a precursor, and prepares SiB6-C-TiO2 composite wires through a liquid-solid phase conversion method, and uses fuse extrusion 3D printing to prepare a composite structure in which flaky TiO2 presents a 'brick laying' structure arrangement, and realizes in-situ generation of flaky TiB2, B4C and SiC phases and formation of a three-dimensional composite structure through reaction pressureless sintering, the grain size is about 100 nm, and each phase is uniformly dispersed, and the generated SiC exists in two phases of alpha-SiC and beta-SiC.
[0029] (3) The application has the advantages of simple process, overcoming the problem that traditional methods cannot realize the forming of special-shaped and large components, flexible regulation of 3D printing process, regulation of the shape, size, phase composition and microstructure of the composite material, and finally improvement of the fracture toughness and bending strength.
[0030] (4) The fracture toughness of the flaky TiB2 toughened B4C-SiC three-dimensional structure composite material prepared by the application is significantly improved, and the fracture toughness can reach 8.2±0.6 MPa·m 1 / 2 At the same time, the bending strength can reach 650±28 MPa. BRIEF DESCRIPTION OF DRAWINGS
[0031] Figure 1 The XRD graph of the flaky TiB2 toughened B4C-SiC composite material prepared in Example 1;
[0032] Figure 2 The SEM graph of the flaky TiB2 toughened B4C-SiC composite material prepared in Example 1;
[0033] Figure 3 The fracture toughness of the flaky TiB2 toughened B4C-SiC composite material prepared in Example 1 and the B4C-SiC composite material prepared in Comparative Example 1;
[0034] Figure 4 The bending strength of the flaky TiB2 toughened B4C-SiC composite material prepared in Example 1 and the B4C-SiC composite material prepared in Comparative Example 1. DETAILED DESCRIPTION
[0035] In order to make the purpose, technical scheme and advantages of the present application clearer, the preferred embodiments of the present application are described in further detail below in combination with examples. All other examples obtained by those of ordinary skill in the art without creative labor based on the examples in the present application belong to the scope of protection of the present application. The SiB6 powder used in the present application is produced by Alpha Epsilon Company, with a particle size of 3-8 μm and a purity of ≥98%; the nano-carbon black is produced by Beijing Ino Kai Technology Co., Ltd., with a particle size of 100 nm and a purity of ≥99.9%; the isopropyl alcohol has a purity of ≥99.8%; the N-methyl-2-pyrrolidone has a purity of ≥99.8%; the ethylene-vinyl acetate copolymer (EVA, brand: Taisox 7470M, purity ≥99%) is produced by Taizhong Synthetic Rubber Industry (Ningbo) Co., Ltd.; the polyether sulfone resin (PES, brand: E3010, purity ≥99%) is produced by Ningbo Dinghang Special Plastic Co., Ltd. The flaky TiO2 powder is prepared by a hydrothermal method, and the specific process is reported in [Jia L, Wang J C, Chen Y, Mo S P, Liu G, Qin G J. Thermo-physical properties of TiO2 / NEPCM nanofluid[J]. Journal of Engineering Thermophysics, 2022, 43(5): 1324-1328.].
[0036] The fuse extrusion 3D printer is a CIUniprint 350 Pro produced by Zhejiang Chaojing Intelligent Technology Co., Ltd.
[0037] Example 1
[0038] The present embodiment provides a preparation method of flaky TiB2 toughened B4C-SiC composite material, and the specific steps are as follows:
[0039] S1, SiB6, nano-carbon black and nano-flaky TiO2 are weighed according to a mass ratio of 50:15:13, mixed uniformly to obtain ceramic aggregate; 100 g of the ceramic aggregate is weighed and then placed in a solvent composed of 120 ml of N-methyl pyrrolidone and 120 ml of isopropyl alcohol, mechanically stirred for 30 min to make it mixed uniformly and defoamed to obtain a ceramic aggregate suspension, which is ready for use;
[0040] S2, ethylene-vinyl acetate copolymer and polyether sulfone resin are weighed according to a mass ratio of 1:1, mixed uniformly to obtain a binder; 22 g of the binder is placed in the ceramic aggregate suspension described in step S1, ultrasonically dispersed for 50 min (wherein the ultrasonic power is 500 W), and mechanically stirred at a temperature of 60 ℃ for 36 h (wherein the stirring speed is 500 r / min) to obtain a ceramic slurry;
[0041] S3, vertically injecting the ceramic slurry into water by using a syringe pump, standing for 8 h for liquid-solid phase conversion, then filtering and naturally drying to obtain ceramic filaments, wherein the injection rate is 5 mL / min and the syringe needle diameter is 4 mm;
[0042] S4, performing fused filament extrusion 3D printing on the ceramic filaments, and cooling after printing to obtain a printed body, wherein the heating temperature during the fused filament extrusion 3D printing is 300 ℃, the printing rate is 10 mm / s, and the printing needle diameter is 500 μm;
[0043] S5, carbonizing and pyrolyzing the printed body at 1200 ℃ for 6 h to sufficiently remove the ethylene-vinyl acetate copolymer and polyether sulfone, wherein the pyrolysis atmosphere is a mixed gas of hydrogen and argon at a volume ratio of 1:9, and the SiB6-C-TiO2 composite material body is obtained after pyrolysis, wherein the heating rate is 8 ℃ / min;
[0044] S6, placing the SiB6-C-TiO2 composite material body into a graphite crucible lined with graphite paper, then heating to 1800 ℃ under the protection of high-purity argon atmosphere, and sintering for 5 h, and cooling after sintering, wherein the heating rate and the cooling rate are both 50 ℃ / min, to obtain a sheet-shaped TiB2-toughened B4C-SiC composite material with a density of 98 % and a fracture toughness of 8.2±0.6 MPa·m 1 / 2 The bending strength can reach 650±28 MPa.
[0045] Example 2
[0046] The embodiment provides a preparation method of a sheet-shaped TiB2-toughened B4C-SiC composite material, and the specific steps are as follows:
[0047] S1, taking SiB6, nano-carbon black and nano-sheet-shaped TiO2 according to a mass ratio of 25:50:10, mixing uniformly to obtain ceramic aggregates; taking 100 g of the ceramic aggregates, and then placing the ceramic aggregates in a solvent composed of 195 ml of N-methyl pyrrolidone and 65 ml of isopropyl alcohol, and mechanically stirring for 40 min to uniformly mix and deaerate to obtain a ceramic aggregate suspension, which is used as needed;
[0048] S2, taking ethylene-vinyl acetate copolymer and polyether sulfone resin according to a mass ratio of 1:2, mixing uniformly to obtain a bonding agent; taking 15 g of the bonding agent and placing the bonding agent in the ceramic aggregate suspension described in step S1, and ultrasonically dispersing for 100 min (wherein the ultrasonic power is 600 W), and mechanically stirring at 70 ℃ for 48 h (wherein the stirring speed is 550 r / min) to obtain a ceramic slurry;
[0049] S3, vertically injecting the ceramic slurry into water by using a syringe pump, standing for 10 h for liquid-solid phase conversion, then filtering and naturally drying to obtain ceramic filaments, wherein the injection rate is 8.0 ml / min and the syringe needle diameter is 6 mm;
[0050] S4, performing fused filament extrusion 3D printing on the ceramic filaments, and cooling after printing to obtain a printed body, wherein the heating temperature during the fused filament extrusion 3D printing is 350 ℃, the printing rate is 15 mm / s, and the printing needle diameter is 800 μm;
[0051] S5, carbonizing and pyrolyzing the printed body at 1300 ℃ for 8 h to sufficiently remove the ethylene-vinyl acetate copolymer and polyether sulfone, wherein the pyrolysis atmosphere is a mixed gas of hydrogen and argon at a volume ratio of 1:9, and the SiB6-C-TiO2 composite material body is obtained after pyrolysis, wherein the heating rate is 10 ℃ / min;
[0052] S6, placing the SiB6-C-TiO2 composite material body into a graphite crucible lined with graphite paper, and then heating to 1900 ℃ under the protection of high-purity argon atmosphere, and sintering for 6 h, and cooling after sintering, wherein the heating rate and the cooling rate are both 80 ℃ / min, to obtain a sheet-shaped TiB2 toughened B4C-SiC composite material with a density of 99 %, and the fracture toughness can reach 6.2±0.5 MPa·m 1 / 2 The bending strength can reach 610±32 MPa.
[0053] Example 3
[0054] The embodiment provides a preparation method of a sheet-shaped TiB2 toughened B4C-SiC composite material, and the specific steps are as follows:
[0055] S1, weighing SiB6, nano-carbon black and nano-sheet-shaped TiO2 according to a mass ratio of 10:22:30, mixing uniformly to obtain ceramic aggregates; weighing 100 g of the ceramic aggregates, and then placing the ceramic aggregates in a solvent composed of 149 ml of N-methyl pyrrolidone and 37 ml of isopropyl alcohol, and mechanically stirring for 80 min to make the ceramic aggregates uniformly mixed and defoamed to obtain a ceramic aggregate suspension, which is used as needed;
[0056] S2, weighing ethylene-vinyl acetate copolymer and polyether sulfone resin according to a mass ratio of 1:2, mixing uniformly to obtain a bonding agent, weighing 38 g of the bonding agent, and placing the bonding agent in the ceramic aggregate suspension obtained in step S1, and performing ultrasonic dispersion treatment for 80 min (wherein the ultrasonic power is 800 W), and then mechanically stirring at a temperature of 80 ℃ for 24 h (wherein the stirring speed is 600 r / min) to obtain a ceramic slurry;
[0057] S3, vertically injecting the ceramic slurry into water by using a syringe pump, and standing for 12 h for liquid-solid phase conversion, then filtering and naturally drying to obtain a ceramic filament, for standby, wherein the injection rate is 3.0 ml / min, and the syringe needle hole diameter is 4 mm;
[0058] S4, performing fused filament extrusion 3D printing on the ceramic filament, and cooling after printing to obtain a printed body, wherein the heating temperature during the fused filament extrusion 3D printing process is 280 ℃, the printing rate is 18 mm / s, and the printing needle diameter is 1000 μm;
[0059] S5, carbonizing and pyrolyzing the printed body after being heated to 1000 ℃ for 4 h to sufficiently remove ethylene-vinyl acetate copolymer and polyether sulfone, wherein the pyrolysis atmosphere is a mixed gas of hydrogen and argon at a volume ratio of 1:9, and the SiB6-C-TiO2 composite material body is obtained after pyrolysis, wherein the heating rate is 5 ℃ / min;
[0060] S6, loading the SiB6-C-TiO2 composite material body into a graphite crucible coated with graphite paper, and then heating to 2000 ℃ under the protection of high-purity argon atmosphere, and sintering for 2 h, and cooling after sintering, wherein the heating rate and the cooling rate are both 100 ℃ / min, to obtain a sheet-shaped TiB2-toughened B4C-SiC composite material with a density of 97 %, and a fracture toughness of 5.2±0.7 MPa·m 1 / 2 The bending strength can reach 620±34 MPa.
[0061] Comparative Example 1
[0062] Referring to the method of Example 1, the only difference is that the ceramic aggregate used is composed of SiB6 and nano-carbon black at a mass ratio of 50:15, i.e. no nano-sheet TiO2 is used, and the other parameters are the same as those of Example 1, to obtain a preparation method of a B4C-SiC composite material. It is detected that the density of the B4C-SiC composite material is 90 %, and the fracture toughness is only 4.0±0.5 MPa·m 1 / 2 , and the bending strength is only 560±35 MPa.
[0063] The density, fracture toughness and bending strength of the composite materials prepared in Example 1 and Comparative Example 1 are shown in Table 1.
[0064]
[0065] From the above comparisons, it can be concluded that:
[0066] (1) The nanosheet TiB2 is introduced in the B4C-SiC composite material in Example 1 to provide crack deflection, crack bridging, crack tip pinning and other toughening approaches, and the fracture toughness and bending strength of the composite material are greatly improved;
[0067] (2) The nanosheet TiO2 is introduced in Example 1 as a template agent and a reaction raw material to participate in the carbon-boron thermal reduction reaction sintering, effectively improving the carbon-boron thermal reduction reaction activity of the SiB6, nanocarbon black, ethylene-vinyl acetate copolymer and polyether sulfone resin reaction system from the aspects of chemical reaction thermodynamics and sintering kinetics, improving the reaction sintering rate, realizing the sintering densification of the sheet TiB2 toughened B4C-SiC composite material, and the sintering density can reach 98%;
[0068] (3) The nanosheet TiO2 introduced in Example 1 can occur carbon-boron thermal reduction reaction with the active pyrolytic carbon generated after pyrolysis of the ethylene-vinyl acetate copolymer and polyether sulfone resin in the mixed binder and SiB6, and the pyrolytic carbon is consumed, otherwise the generation of the pyrolytic carbon will prevent the sintering densification of the composite material and reduce the density thereof. The density of the composite material in Comparative Example 1 is only 90%, and a large number of pores and other defects are introduced, which greatly reduces the fracture toughness and bending strength of the composite material.
[0069] The above-described embodiments are part of the embodiments of the present application, rather than all the embodiments. The detailed description of the embodiments of the present application is not intended to limit the scope of the claimed application, but only represents selected embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative labor are within the scope of protection of the present application.
Claims
1. A sheet-like TiB2-toughened B4C-SiC composite material, characterized in that, It includes ceramic aggregate and binder; the ceramic aggregate is composed of SiB6, nano carbon black and nano-sheet TiO2; the binder is a mixture of ethylene-vinyl acetate copolymer and polyethersulfone resin; The mass ratio of SiB6, nano carbon black, and nano-sheet TiO2 is 5~50:10~75:1~30; The mass ratio of the ethylene-vinyl acetate copolymer to the polyethersulfone resin is 1:1~2; The binder accounts for 10% to 40% of the mass of the ceramic aggregate.
2. The method for preparing the sheet-like TiB2-toughened B4C-SiC composite material as described in claim 1, characterized in that, Includes the following steps: S1. Weigh out SiB6, carbon black, and flake TiO2 in proportion, mix them, place them in a solvent, stir mechanically until uniform, and degas to obtain a ceramic aggregate suspension for later use. S2. Ethylene-vinyl acetate copolymer and polyethersulfone resin are added to the ceramic aggregate suspension in proportion. After ultrasonic dispersion treatment for 30~120 min, the mixture is mechanically stirred at a temperature of 50 ℃~80 ℃ for 24~60 h to obtain ceramic slurry. S3. Use an injection pump to vertically inject the ceramic slurry into water, let it stand for 6 h to 12 h to carry out liquid-solid phase conversion, then filter and air dry to obtain ceramic wire material for later use. S4. The ceramic filament is fused and extruded for 3D printing. After printing, it is cooled to obtain a printed blank. S5. The printed blank is heated to 800 ℃~1400 ℃ and then subjected to carbonization pyrolysis, wherein the pyrolysis atmosphere is a mixture of hydrogen and argon gas, and after the pyrolysis is completed, a SiB6-C-TiO2 composite material blank is obtained. S6. The SiB6-C-TiO2 composite material preform is heated to 1600 ℃~2000 ℃ under inert atmosphere protection, and sintered for 1 h~6 h. After sintering, it is cooled to obtain a sheet-like TiB2 toughened B4C-SiC composite material.
3. The method for preparing a sheet-like TiB2-toughened B4C-SiC composite material as described in claim 2, characterized in that, The solvent is a mixture of N-methylpyrrolidone and isopropanol.
4. The method for preparing a sheet-like TiB2-toughened B4C-SiC composite material as described in claim 2, characterized in that, In step S2, the ultrasonic power is 300 W to 1000 W, and the mechanical stirring speed is 300 r / min to 600 r / min.
5. The method for preparing a sheet-like TiB2-toughened B4C-SiC composite material as described in claim 2, characterized in that, In step S3, the injection rate is 2.5 mL / min to -8.0 mL / min, and the syringe needle diameter is 2 mm to 8 mm.
6. The method for preparing a sheet-like TiB2-toughened B4C-SiC composite material as described in claim 2, characterized in that, In step S4, the heating temperature in fused filament extrusion 3D printing is 200 ℃~400 ℃, and the printing speed is 4.0 mm / s~20 mm / s.
7. The method for preparing a sheet-like TiB2-toughened B4C-SiC composite material as described in claim 2, characterized in that, In step S5, the volume ratio of hydrogen to argon is 1:9, the heating rate is 5 ℃ / min~10 ℃ / min, and the carbonization pyrolysis time is 2 h-8 h.
8. The method for preparing a sheet-like TiB2-toughened B4C-SiC composite material as described in claim 2, characterized in that, In step S6, the inert atmosphere is argon.
9. The method for preparing a sheet-like TiB2-toughened B4C-SiC composite material as described in claim 2, characterized in that, In step S6, the heating and cooling rates are both 20 ℃ / min to 100 ℃ / min.
Citation Information
Patent Citations
METHOD FOR SYNTHESIZING A TITANIUM DIBORIDE POWDER
FR3127754A3
Ablation-resistant high-entropy carbide-high-entropy diboride-silicon carbide multiphase ceramic and preparation thereof
US20230167029A1