CN117584565B - Multilayer structure silicon carbide wave-absorbing material and preparation method thereof - Google Patents
Multilayer structure silicon carbide wave-absorbing material and preparation method thereofInfo
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- CN117584565B CN117584565B CN202311493354.XA CN202311493354A CN117584565B CN 117584565 B CN117584565 B CN 117584565B CN 202311493354 A CN202311493354 A CN 202311493354A CN 117584565 B CN117584565 B CN 117584565B
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Abstract
The invention provides a multilayer structure silicon carbide wave-absorbing material and a preparation method thereof, wherein the multilayer structure silicon carbide wave-absorbing material comprises a first plane layer, a first circular tube layer, a second plane layer, a second circular tube layer and a third plane layer which are sequentially stacked, the first circular tube layer and the second circular tube layer comprise a plurality of hollow circular tubes which are arranged in parallel, adjacent hollow circular tubes are abutted against each other, and the multilayer structure silicon carbide wave-absorbing material comprises the following raw materials, by mass, 40% -80% of silicon carbide powder, 10% -40% of paraffin, 5% -10% of thermoplastic resin, 1% -5% of stearic acid and 1% -5% of sintering aid. The invention improves the composition and structure of the raw materials of the silicon carbide material, widens the wave absorbing frequency band of the material and improves the mechanical property by adjusting the thermoplastic resin, and the material has a multi-layer structure, and two layers of hollow round tubes are arranged at intervals, so that the wave absorbing property of the material can be improved.
Description
Technical Field
The invention relates to the technical field of preparation of wave-absorbing materials, in particular to a silicon carbide wave-absorbing material and a preparation method thereof.
Background
With the rapid development of the technology of aerospace aircrafts, higher requirements are put on protective materials and structures on the surfaces of aircrafts, so that materials integrating functions of light weight, bearing, broadband, high-efficiency wave absorption and the like are required to be developed urgently. The silicon carbide ceramic material is a typical covalent compound, has the advantages of low density, high heat conductivity coefficient, small thermal expansion coefficient, good chemical stability, high mechanical strength and the like, and is a high-temperature-resistant and corrosion-resistant material with great development prospect, but the silicon carbide material has lower conductivity and dielectric loss and is unfavorable for electromagnetic wave absorption.
In recent years, various researches show that structures of different levels have a superposition effect on wave absorbing capacity, and the wave absorbing performance of the material can be effectively improved, so that the wave absorbing performance of the silicon carbide material can be improved theoretically through composite or structural design.
Silicon carbide is a compound with extremely strong covalent bond, has the characteristics of high hardness, insulation and high temperature resistance, and cannot be processed by adopting traditional methods such as pressure processing, cutting processing, wire-cut electric discharge machining and the like. At present, a processing method only comprises a diamond grinding wheel, but the method has high grinding processing cost and long period, so that the preparation of a silicon carbide ceramic piece with a large-size and complex-shape structure is very difficult, the space structure of a silicon carbide material cannot be effectively regulated and controlled, and the development of the silicon carbide wave-absorbing material is limited.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to solve the technical problem of how to regulate and control the space structure of the silicon carbide material and improve the wave absorbing performance of the silicon carbide material.
In order to solve the problems, the invention provides a multilayer structure silicon carbide wave-absorbing material, which comprises a first planar layer, a first circular tube layer, a second planar layer, a second circular tube layer and a third planar layer which are sequentially stacked, wherein the first circular tube layer and the second circular tube layer comprise a plurality of hollow circular tubes which are arranged in parallel, adjacent hollow circular tubes are propped against each other, and the multilayer structure silicon carbide wave-absorbing material comprises the following raw materials, by mass, 40% -80% of silicon carbide powder, 10% -40% of paraffin, 5% -10% of thermoplastic resin, 1% -5% of stearic acid and 1% -5% of sintering aid.
The invention improves the silicon carbide material in raw materials and structure, can improve the mechanical property of the material by adjusting the content of organic matters, has a multi-layer structure, and is provided with two layers of hollow round tubes at intervals, so that the reflection and refraction can continuously occur in different directions in the wave propagation process, thereby reducing the wave propagation energy and improving the wave absorption performance of the material.
Further, the thickness of the first plane layer is 0.5-1 mm, the thickness of the first circular tube layer is 0.5-1 mm, the thickness of the second plane layer is 0.5-1 mm, the thickness of the second circular tube layer is 0.5-1 mm, and the thickness of the third plane layer is 0.5-1 mm. By controlling the thickness of each layer in the composite material, the mechanical property and the wave absorbing property of the material can be adjusted.
Further, the outer diameter of the hollow round tube is 0.5-1 mm, and the wall thickness is 0.1-0.2 mm.
Further, the thermoplastic resin is selected from any one or more of polylactic acid, ABS, polycarbonate, nylon, polyethylene, ethylene vinyl acetate polymer, and the like. And a high polymer with good bonding performance is selected, so that the wire rod forming is facilitated.
Further, the sintering aid is selected from any one or more of aluminum, silicon, aluminum oxide, yttrium oxide and carbon black.
Further, the particle size of the silicon carbide powder and the sintering aid is 200-400 meshes, and the particle size of the thermoplastic resin is more than 100 meshes.
The invention also provides a preparation method of the silicon carbide wave-absorbing material with the multilayer structure, which comprises the following steps:
s1, mixing and granulating, namely placing silicon carbide powder, a sintering aid and stearic acid into a ball mill, uniformly mixing, drying, uniformly mixing with thermoplastic resin and paraffin in an internal mixer, and crushing to obtain mixed particles with the particle size of 50-500 mu m;
S2, extruding into wires, namely adding the dried mixed particles into a melt extrusion molding machine, conveying the powder forwards under the action of a screw, melt mixing, and extrusion molding to obtain silicon carbide/thermoplastic resin composite wires;
s3, printing and forming, namely placing the silicon carbide/thermoplastic resin composite wire into 3D printing equipment, adjusting equipment parameters, printing under the control of a computer, and printing the biscuit in a layering and solidifying mode and a layering and overlapping mode;
S4, degreasing, namely degreasing the printed biscuit to obtain a preform;
s5, sintering, namely placing the preform in a sintering furnace, and sintering at high temperature to obtain the silicon carbide wave-absorbing material with the multilayer structure.
According to the preparation method, a fused deposition 3D printing forming process is adopted, the ceramic raw material is preprocessed through a mixing granulation step, so that the silicon carbide/thermoplastic resin composite wire compatible with common 3D printing equipment is obtained, the silicon carbide with the hollow round tube and the multilayer structure is successfully prepared, the design and the rapid manufacturing of the complex structure are realized, the special high-temperature fused 3D printing equipment is not needed, the production efficiency is improved, and the cost is saved.
Further, in the step S1, the ball milling speed is 200-400 r/min, the drying temperature is 50-80 ℃, the banburying temperature is 120-180 ℃ and the rotating speed is 15-40 r/min.
Further, in the step S2, the screw speed of the melt extrusion molding machine is 10-20 r/min, the temperature of the preheating zone is 120-140 ℃, the melt mixing temperature is 140-150 ℃, and the silicon carbide/thermoplastic resin composite wire rod with the millimeter-grade diameter can be obtained through mixing and extrusion molding in the step S1.
Further, in the step S3, the temperature of a spray head of the 3D printing equipment is controlled to be 100-200 ℃, the temperature of an objective table is controlled to be 20-150 ℃, the printing speed is 10-50 mm/S, the single-layer thickness is 0.1-0.2 mm, and the ceramic/polymer blank is obtained in a layered solidification and layer-by-layer superposition mode.
Further, the concrete process of the step S4 is that the biscuit is heated to 150-250 ℃ in a degreasing furnace at a heating rate of 1-5 ℃ per minute, then heated to 500-700 ℃ at a heating rate of 0.2-1 ℃ per minute, and the temperature is kept for 1-2 hours, so that a preform is obtained. The production efficiency can be improved by adopting a distributed heating mode, the heating speed of the second stage is slowed down, and cracking is avoided in the process of degreasing the biscuit.
Further, the specific process of the step S5 is that the prefabricated body is placed in a sintering furnace, the prefabricated body is heated to 1900-2200 ℃ at the temperature rising rate of 2-5 ℃ per minute, and the temperature is kept for 1-3 hours, so that the silicon carbide wave-absorbing material with the multilayer structure is obtained. And degreasing and sintering to obtain the high-precision silicon carbide wave-absorbing material with excellent performance.
Drawings
FIG. 1 is a schematic structural diagram of a multi-layer silicon carbide wave-absorbing material embodying the method of the present invention;
FIG. 2 is a side view of a multilayer structure silicon carbide wave absorbing material embodying the method of the present invention;
FIG. 3 is a scanning electron microscope image of a silicon carbide wave-absorbing material obtained in embodiment 1 of the present invention;
FIG. 4 is a scanning electron microscope image of a silicon carbide wave-absorbing material obtained in embodiment 1 of the present invention;
FIG. 5 is a graph showing the absorption of a silicon carbide wave-absorbing material obtained in example 1 of the present invention.
Reference numerals illustrate:
1-a first plane layer, 2-a first circular tube layer, 3-a second plane layer, 4-a second circular tube layer and 5-a third plane layer.
Detailed Description
In order that the above objects, features and advantages of the invention will be readily understood, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings. It should be noted that the following examples are only for illustrating the implementation method and typical parameters of the present invention, and are not intended to limit the scope of the parameters described in the present invention, so that reasonable variations are introduced and still fall within the scope of the claims of the present invention.
It should be noted that endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and that such range or value should be understood to include values approaching such range or value. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
Referring to fig. 1 and fig. 2, an embodiment of the present invention provides a silicon carbide wave absorbing material with a multilayer structure, which includes a first planar layer 1, a first circular tube layer 2, a second planar layer 3, a second circular tube layer 4 and a third planar layer 5 that are sequentially stacked, where the first circular tube layer 2 and the second circular tube layer 4 include a plurality of hollow circular tubes arranged in parallel, and adjacent hollow circular tubes are abutted against each other. The material has a multi-layer structure, and two layers of hollow round tubes are arranged at intervals, so that the quality of the material can be reduced, and the wave absorbing performance of the material can be improved.
The thickness of the first plane layer 1 is 0.5-1 mm, the thickness of the first round tube layer 2 is 0.5-1 mm, the thickness of the second plane layer 3 is 0.5-1 mm, the thickness of the second round tube layer 4 is 0.5-1 mm, the thickness of the third plane layer 5 is 0.5-1 mm, and the thicknesses of the plane layers and the round tube layers can be the same or different. Preferably, the outer diameter of the hollow round tube in the round tube layer is 0.5-1 mm, and the wall thickness is 0.1-0.2 mm.
The raw materials of the silicon carbide wave-absorbing material mainly comprise silicon carbide powder and thermoplastic resin, wherein the thermoplastic resin is selected from polylactic acid, ABS, polycarbonate, nylon, polyethylene, ethylene vinyl acetate polymer and the like. Preferably, the particle size of the silicon carbide powder is 200-400 meshes, and the particle size of the thermoplastic resin is more than 100 meshes.
The silicon carbide wave-absorbing material is prepared by adopting a fused deposition 3D printing forming process, and the specific preparation method comprises the following steps:
S1, mixing and granulating, namely, placing 40% -80% of silicon carbide powder, 1% -5% of stearic acid and 1% -5% of sintering aid in a ball mill, uniformly mixing, drying, then uniformly mixing with 10% -40% of paraffin and 5% -10% of thermoplastic resin in an internal mixer, and crushing to obtain mixed particles with the particle size of 50-500 mu m. In the specific embodiment, the mixing process comprises the steps of sequentially placing silicon carbide powder, stearic acid and sintering aid in a ball mill according to the proportion, uniformly mixing, and drying, wherein the ball milling speed is 200-400 r/min, and the drying temperature is 50-80 ℃. And then placing the mixture, the thermoplastic resin and the paraffin into an internal mixer for internal mixing at the temperature of 120-180 ℃ at the rotating speed of 15-40 r/min for 1-5 h. After the mixing is completed, the mixture is crushed by a jaw crusher to obtain particles with the particle size of 50-500 mu m.
S2, extruding into wires, namely adding the dried mixed particles into a melt extrusion molding machine, conveying the powder forwards under the action of a screw, melt mixing, and extruding and molding to obtain the silicon carbide/thermoplastic resin composite wires. In the specific embodiment, the screw speed of the melt extrusion molding machine is 10-20 r/min, the temperature of the preheating zone is 120-140 ℃, the melt mixing temperature is 140-150 ℃, and the silicon carbide/thermoplastic resin composite wire with millimeter-grade diameter can be obtained through mixing and extrusion molding in the step.
S3, printing and forming, namely placing the silicon carbide/thermoplastic resin composite wire into 3D printing equipment, adjusting equipment parameters, printing under the control of a computer, and printing the biscuit in a layering solidification and layering superposition mode. In the specific embodiment, the temperature of a spray head of the 3D printing equipment is controlled to be 100-200 ℃, the temperature of an objective table is controlled to be 20-150 ℃, the printing speed is 10-50 mm/s, and the single-layer thickness is 0.1-0.2 mm.
And S4, degreasing, namely degreasing the printed biscuit to obtain a preform. In the specific embodiment, the biscuit is heated to 150-250 ℃ in a degreasing furnace at a temperature rising rate of 5-10 ℃ per minute, then heated to 500-700 ℃ at a temperature rising rate of 0.2-1 ℃ per minute, and kept for 1-2 hours to finish degreasing.
S5, sintering, namely placing the preform in a sintering furnace, and sintering at high temperature to obtain the silicon carbide wave-absorbing material with the multilayer structure. In a specific embodiment, the preform is heated to 1900-2200 ℃ in a sintering furnace at a heating rate of 2-5 ℃ per minute, and is kept for 1-3 hours, and the sintering process is finished.
The preparation method successfully prepares the silicon carbide wave-absorbing material with the multilayer structure by using the fused deposition 3D printing forming process, has simple equipment and short production period, gets rid of the restriction of mold forming, improves the production efficiency, saves the cost and can realize high-efficiency and batch preparation of the wave-absorbing material.
The technical scheme and effect of the present invention are described below by specific examples. The performance test methods adopted in the following examples are as follows, the material density test method refers to GB/T25995-2010 fine ceramic density and apparent porosity test method, and the material flexural strength test method refers to GB/T6569-2006 fine ceramic flexural strength test method.
Example 1
The design of the multi-layer structure silicon carbide wave absorbing material comprises a first plane layer, a first circular tube layer, a second plane layer, a second circular tube layer and a third plane layer which are sequentially laminated, wherein the first circular tube layer and the second circular tube layer comprise a plurality of hollow circular tubes which are arranged in parallel, and adjacent hollow circular tubes are propped against each other. The thickness of the first plane layer is 1mm, the thickness of the first circular tube layer is 1mm, the thickness of the second plane layer is 1mm, the thickness of the second circular tube layer is 1mm, the thickness of the third plane layer is 1mm, the outer diameter of the hollow circular tube in the circular tube layer is 1mm, and the wall thickness is 0.1mm.
The preparation process of the silicon carbide wave-absorbing material comprises the following steps:
Mixing and granulating, namely uniformly mixing 76% of silicon carbide powder, 3% of stearic acid and 2% of carbon black in a ball mill, drying, then mixing with 16% of paraffin and 3% of thermoplastic resin in an internal mixer, wherein the internal mixing temperature is 160 ℃, the rotating speed is 25r/min, the time is 3h, and then crushing to obtain mixed particles with the particle size of about 50-500 mu m.
Extruding into wire rod, adding the dried mixed particles into a melt extrusion molding machine, controlling the rotating speed of a screw rod to be 20r/min, controlling the temperature of a preheating zone to be 130 ℃, controlling the temperature of melt mixing to be 160 ℃, and extruding and molding to obtain the silicon carbide/thermoplastic resin composite wire rod with the diameter of 1.75+/-0.05 mm.
And (3) printing and forming, namely placing the silicon carbide/thermoplastic resin composite wire into 3D printing equipment, controlling the temperature of a spray head to be 180 ℃, controlling the temperature of an objective table to be 50 ℃, controlling the printing speed to be 20mm/s and the single-layer thickness to be 0.1mm, and printing the biscuit in a layering and solidifying mode and a layering and overlapping mode.
And S4, degreasing, namely putting the printed biscuit into a degreasing furnace, heating to 200 ℃ at a temperature rising rate of 5 ℃ per minute, then heating to 600 ℃ at a temperature rising rate of 10 ℃ per hour, and preserving heat for 1 hour to finish degreasing to obtain the preform.
S5, sintering, namely placing the preform in a sintering furnace, heating to 2000 ℃ at a temperature rising rate of 5 ℃ per minute, and preserving heat for 2 hours to obtain the silicon carbide wave-absorbing material with a designed structure, wherein the material structure is shown in fig. 3 and 4, and the material is compact.
S6, wave-absorbing test, namely printing out wave-absorbing test samples in different wave bands from the prepared structural silicon carbide wave-absorbing material through fused deposition, and testing the wave-absorbing performance in the X wave band of 8.2-12.4 GHz.
The density of the silicon carbide wave-absorbing material is 3.15g/cm 3, the bending strength is 220MPa, and as can be seen from fig. 5, the silicon carbide material with the multilayer structure has excellent wave-absorbing performance, and the minimum reflection loss of the silicon carbide wave-absorbing material in the X wave band is-19.8 dB.
Example 2
The design of the multi-layer structure silicon carbide wave absorbing material comprises a first plane layer, a first circular tube layer, a second plane layer, a second circular tube layer and a third plane layer which are sequentially laminated, wherein the first circular tube layer and the second circular tube layer comprise a plurality of hollow circular tubes which are arranged in parallel, and adjacent hollow circular tubes are propped against each other. The thickness of the first plane layer is 0.5mm, the thickness of the first circular tube layer is 1mm, the thickness of the second plane layer is 1mm, the thickness of the second circular tube layer is 1mm, the thickness of the third plane layer is 0.5mm, the outer diameter of the hollow circular tube in the circular tube layer is 1mm, and the wall thickness is 0.2mm.
The preparation process of the silicon carbide wave-absorbing material comprises the following steps:
Granulating, namely placing 60% of silicon carbide powder, 5% of stearic acid and 5% of carbon black into a ball mill, uniformly mixing, drying, then placing into an internal mixer together with 25% of paraffin and 5% of thermoplastic resin, banburying at 180 ℃ at the rotating speed of 20r/min for 2 hours, and crushing to obtain mixed particles with the particle size of about 50-500 mu m.
Mixing into wire rod, adding the dried mixed particles into a melt extrusion molding machine, controlling the rotating speed of a screw rod to be 10r/min, controlling the temperature of a preheating zone to be 120 ℃, controlling the temperature of melt mixing to be 140 ℃, and extruding and molding to obtain the silicon carbide/thermoplastic resin composite wire rod with the diameter of 1.75+/-0.05 mm.
And (3) printing and forming, namely placing the silicon carbide/thermoplastic resin composite wire into 3D printing equipment, controlling the temperature of a spray head to be 170 ℃, controlling the temperature of an objective table to be 80 ℃, controlling the printing speed to be 30mm/s and the single-layer thickness to be 0.2mm, and printing the biscuit in a layering and solidifying mode and a layering and overlapping mode.
And S4, degreasing, namely putting the printed biscuit into a degreasing furnace, heating to 250 ℃ at the heating rate of 10 ℃ per minute, then heating to 700 ℃ at the heating rate of 10 ℃ per hour, and preserving heat for 1h to finish degreasing to obtain the preform.
S5, sintering, namely placing the preform in a sintering furnace, heating to 1900 ℃ at a heating rate of 2 ℃ per min, and preserving heat for 3 hours to obtain the silicon carbide wave-absorbing material with the designed structure.
The silicon carbide material was tested to have a density of 3.06g/cm 3 and a flexural strength of 183MPa, with a minimum reflection loss of-18.4 dB in the X-band.
Example 3
The design of the multi-layer structure silicon carbide wave absorbing material comprises a first plane layer, a first circular tube layer, a second plane layer, a second circular tube layer and a third plane layer which are sequentially laminated, wherein the first circular tube layer and the second circular tube layer comprise a plurality of hollow circular tubes which are arranged in parallel, and adjacent hollow circular tubes are propped against each other. The thickness of the first plane layer is 1mm, the thickness of the first round tube layer is 0.8mm, the thickness of the second plane layer is 0.6mm, the thickness of the second round tube layer is 0.8mm, the thickness of the third plane layer is 1mm, the outer diameter of the hollow round tube in the round tube layer is 0.8mm, and the wall thickness is 0.1mm.
The preparation process of the silicon carbide wave-absorbing material comprises the following steps:
And (3) banburying granulation, namely placing 70% of silicon carbide powder, 3% of stearic acid, 5% of aluminum oxide and yttrium oxide into a ball mill, uniformly mixing, drying, placing the mixture, 17% of paraffin and 5% of thermoplastic resin into an internal mixer, banburying at 185 ℃ for 3 hours at 15r/min, and crushing to obtain mixed particles with the particle size of about 50-500 mu m.
Extruding into wire rod, adding the dried mixed particles into a melt extrusion molding machine, controlling the rotating speed of a screw rod to be 15r/min, controlling the temperature of a preheating zone to be 120 ℃, controlling the temperature of melt mixing to be 150 ℃, and extruding and molding to obtain the silicon carbide/thermoplastic resin composite wire rod with the diameter of 1.75+/-0.05 mm.
And (3) printing and forming, namely placing the silicon carbide/thermoplastic resin composite wire into 3D printing equipment, controlling the temperature of a spray head to be 150 ℃, controlling the temperature of an objective table to be 40 ℃, controlling the printing speed to be 80mm/s and the single-layer thickness to be 0.1mm, and printing the biscuit in a layering and solidifying mode and a layering and overlapping mode.
And S4, degreasing, namely putting the printed biscuit into a degreasing furnace, heating to 200 ℃ at a temperature rising rate of 5 ℃ per minute, then heating to 600 ℃ at a temperature rising rate of 10 ℃ per hour, and preserving heat for 2 hours to finish degreasing to obtain the preform.
S5, sintering, namely placing the preform in a sintering furnace, heating to 2100 ℃ at a temperature rising rate of 5 ℃ per minute, and preserving heat for 2 hours to obtain the silicon carbide wave-absorbing material with the designed structure.
The silicon carbide material was tested to have a density of 3.13g/cm 3 and a flexural strength of 204MPa with a minimum reflection loss in the X-band of-17.6 dB.
Example 4
The design of the multi-layer structure silicon carbide wave absorbing material comprises a first plane layer, a first circular tube layer, a second plane layer, a second circular tube layer and a third plane layer which are sequentially laminated, wherein the first circular tube layer and the second circular tube layer comprise a plurality of hollow circular tubes which are arranged in parallel, and adjacent hollow circular tubes are propped against each other. The thickness of the first plane layer is 0.8mm, the thickness of the first round tube layer is 0.5mm, the thickness of the second plane layer is 1mm, the thickness of the second round tube layer is 0.8mm, the thickness of the third plane layer is 1mm, the outer diameter of the hollow round tube in the round tube layer is 0.5mm, and the wall thickness is 0.1mm.
The preparation process of the silicon carbide wave-absorbing material comprises the following steps:
And (3) banburying granulation, namely placing 67% of silicon carbide powder, 1% of stearic acid and 4% of aluminum oxide into a ball mill, uniformly mixing, drying, then placing the mixture, 25% of paraffin and 3% of thermoplastic resin into an internal mixer for banburying at 160 ℃ at a rotating speed of 30r/min for 4 hours, and crushing to obtain mixed particles with the particle size of about 50-500 mu m.
Mixing to obtain wire rod, adding the dried mixed particles into a melt extrusion molding machine, controlling the rotation speed of a screw to be 10r/min, controlling the temperature of a preheating zone to be 130 ℃, controlling the temperature of melt mixing to be 150 ℃, and extruding and molding to obtain the silicon carbide/thermoplastic resin composite wire rod with the diameter of 1.75+/-0.05 mm.
And (3) printing and forming, namely placing the silicon carbide/thermoplastic resin composite wire into 3D printing equipment, controlling the temperature of a spray head to be 170 ℃, controlling the temperature of an objective table to be 60 ℃, controlling the printing speed to be 30mm/s and the single-layer thickness to be 0.1mm, and printing the biscuit in a layering and solidifying mode and a layering and overlapping mode.
And S4, degreasing, namely putting the printed biscuit into a degreasing furnace, heating to 200 ℃ at a temperature rising rate of 5 ℃ per minute, then heating to 650 ℃ at a temperature rising rate of 10 ℃ per hour, and preserving heat for 2 hours to finish degreasing to obtain the preform.
S5, sintering, namely placing the preform in a sintering furnace, heating to 2200 ℃ at a temperature rising rate of 5 ℃ per minute, and preserving heat for 1.5 hours to obtain the silicon carbide wave-absorbing material with the designed structure.
The density of the silicon carbide material was tested to be 3.09g/cm 3, the flexural strength was 189MPa, and the minimum reflection loss in the X-band was-19 dB.
Comparative example 1
A silicon carbide wave-absorbing material of a single-layer structure was prepared, the thickness of which was 5mm, and the raw materials and the process for preparing the same as in example 1.
The density of the silicon carbide material is 3.16g/cm 3, the bending strength is 245MPa, and the minimum reflection loss of the silicon carbide material in the X wave band is-14 dB.
Comparative example 2
The method for preparing the silicon carbide wave-absorbing material with the multilayer structure comprises a first plane layer, a first round tube layer and a second plane layer which are sequentially laminated. The thickness of the first plane layer is 1.5mm, the thickness of the first round tube layer is 1mm, the thickness of the second plane layer is 1.5mm, the outer diameter of the hollow round tube in the round tube layer is 1mm, and the wall thickness is 0.2mm.
The preparation raw materials and the process are the same as in example 2.
The silicon carbide material was tested to have a density of 3.15g/cm 3 and a flexural strength of 236MPa with a minimum reflection loss in the X-band of-15.7 dB.
Although the present invention is disclosed above, the present invention is not limited thereto. Various changes and modifications may be made by one skilled in the art without departing from the spirit and scope of the invention, and the scope of the invention should be assessed accordingly to that of the appended claims.
Claims (8)
1. The multilayer structure silicon carbide wave absorbing material is characterized by comprising a first planar layer, a first circular tube layer, a second planar layer, a second circular tube layer and a third planar layer which are sequentially stacked, wherein the first circular tube layer and the second circular tube layer comprise a plurality of hollow circular tubes which are arranged in parallel, adjacent hollow circular tubes are propped against each other, the multilayer structure silicon carbide wave absorbing material comprises the following raw materials, by mass, 40% -80% of silicon carbide powder, 10% -40% of paraffin, 5% -10% of thermoplastic resin, 1% -5% of stearic acid and 1% -5% of sintering aid, the thickness of the first planar layer is 0.5-1 mm, the thickness of the first circular tube layer is 0.5-1 mm, the thickness of the second planar layer is 0.5-1 mm, the thickness of the second circular tube layer is 0.5-1 mm, the thickness of the third planar layer is 0.5-1 mm, the outer diameter of the hollow circular tube is 0.5-1 mm, and the wall thickness is 0.1-2 mm;
the preparation method of the silicon carbide wave-absorbing material with the multilayer structure comprises the following steps:
s1, mixing and granulating, namely placing silicon carbide powder, a sintering aid and stearic acid into a ball mill, uniformly mixing, drying, uniformly mixing with thermoplastic resin and paraffin in an internal mixer, and crushing to obtain mixed particles with the particle size of 50-500 mu m;
S2, extruding into wires, namely adding the dried mixed particles into a melt extrusion molding machine, conveying the powder forwards under the action of a screw, melt mixing, and extrusion molding to obtain silicon carbide/thermoplastic resin composite wires;
s3, printing and forming, namely placing the silicon carbide/thermoplastic resin composite wire into 3D printing equipment, adjusting equipment parameters, printing under the control of a computer, and printing the biscuit in a layering and solidifying mode and a layering and overlapping mode;
S4, degreasing, namely degreasing the printed biscuit to obtain a preform;
s5, sintering, namely placing the preform in a sintering furnace, and sintering at high temperature to obtain the silicon carbide wave-absorbing material with the multilayer structure.
2. The multi-layer silicon carbide wave absorbing material according to claim 1, wherein the thermoplastic resin is selected from any one or more of polylactic acid, ABS, polycarbonate, nylon, polyethylene, ethylene vinyl acetate polymer, and the sintering aid is selected from any one or more of aluminum, silicon, aluminum oxide, yttrium oxide, and carbon black.
3. The multilayered silicon carbide wave absorbing material according to claim 2, wherein the particle size of the silicon carbide powder is 200-400 mesh, and the particle size of the thermoplastic resin is more than 100 mesh.
4. A method for producing the silicon carbide wave-absorbing material having a multilayer structure according to any one of claims 1 to 3, comprising the steps of:
s1, mixing and granulating, namely placing silicon carbide powder, a sintering aid and stearic acid into a ball mill, uniformly mixing, drying, uniformly mixing with thermoplastic resin and paraffin in an internal mixer, and crushing to obtain mixed particles with the particle size of 50-500 mu m;
S2, extruding into wires, namely adding the dried mixed particles into a melt extrusion molding machine, conveying the powder forwards under the action of a screw, melt mixing, and extrusion molding to obtain silicon carbide/thermoplastic resin composite wires;
s3, printing and forming, namely placing the silicon carbide/thermoplastic resin composite wire into 3D printing equipment, adjusting equipment parameters, printing under the control of a computer, and printing the biscuit in a layering and solidifying mode and a layering and overlapping mode;
S4, degreasing, namely degreasing the printed biscuit to obtain a preform;
s5, sintering, namely placing the preform in a sintering furnace, and sintering at high temperature to obtain the silicon carbide wave-absorbing material with the multilayer structure.
5. The method for preparing a silicon carbide wave-absorbing material with a multilayer structure according to claim 4, wherein in the step S1, the ball milling speed is 200-400 r/min, the drying temperature is 50-80 ℃, the banburying temperature is 120-180 ℃ and the rotating speed is 15-40 r/min.
6. The method for preparing a silicon carbide wave-absorbing material with a multilayer structure according to claim 4, wherein in the step S2, the screw speed of the melt extrusion molding machine is 10-20 r/min, the preheating zone temperature is 120-140 ℃, and the melt mixing temperature is 140-150 ℃.
7. The method for preparing the silicon carbide wave-absorbing material with the multilayer structure according to claim 4, wherein in the step S3, the temperature of a spray head of the 3D printing device is controlled to be 100-200 ℃, the temperature of an objective table is controlled to be 20-150 ℃, the printing speed is 10-50 mm/S, and the single-layer thickness is 0.1-0.2 mm.
8. The method for preparing the multilayer structure silicon carbide wave-absorbing material according to claim 4, wherein the step S4 comprises the specific process of heating a biscuit to 150-250 ℃ at a temperature rising rate of 1-5 ℃ per minute in a degreasing furnace, then heating to 500-700 ℃ at a temperature rising rate of 0.2-1 ℃ per minute, and preserving heat for 1-2 hours to obtain a preform, and the step S5 comprises the specific process of placing the preform in a sintering furnace, heating to 1900-2200 ℃ at a temperature rising rate of 2-5 ℃ per minute, and preserving heat for 1-3 hours to obtain the multilayer structure silicon carbide wave-absorbing material.
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