CN115141020A - Preparation method of high-toughness broadband electromagnetic wave absorption super-layered bionic ceramic - Google Patents

Preparation method of high-toughness broadband electromagnetic wave absorption super-layered bionic ceramic Download PDF

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CN115141020A
CN115141020A CN202210774519.XA CN202210774519A CN115141020A CN 115141020 A CN115141020 A CN 115141020A CN 202210774519 A CN202210774519 A CN 202210774519A CN 115141020 A CN115141020 A CN 115141020A
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electromagnetic wave
casting
weight
super
interface layer
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李�权
张建浩
王之成
杨建�
汪洋
潘丽梅
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Nanjing Tech University
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Nanjing Tech University
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Abstract

The invention discloses a preparation method of a super-layered bionic ceramic with high toughness and broadband electromagnetic wave absorption, belonging to the technical field of layered bionic ceramic material preparation, wherein a substrate layer casting sheet and an interface layer casting sheet are alternately laminated, and then the super-layered bionic ceramic material is prepared by cutting, laminating, binder removal, high-temperature sintering and other processes; by controlling the content and distribution of electromagnetic wave absorbent in the substrate layer and the interface layer, the super-layer structure imitation with the characteristics of low-high-low sandwich structure with gradually changed impedance/loss gradient, periodic impedance/loss change or loss is preparedRaw ceramic; the toughness of the ceramic material can be effectively improved by introducing a weak interface, and the toughness can exceed 12 MP.m 1/2 (ii) a Meanwhile, the super-layered bionic ceramic material can obtain broadband wave absorbing performance by optimizing the content and distribution of the electromagnetic wave absorbent, and the prepared ceramic material can be widely applied to advanced stealth equipment.

Description

Preparation method of high-toughness broadband electromagnetic wave absorption super-layered bionic ceramic
Technical Field
The invention belongs to the technical field of preparation of layered bionic ceramic materials, and particularly relates to a preparation method of a super-layered bionic ceramic with functions of broadband electromagnetic wave absorption, high toughness and the like.
Background
The wave-absorbing ceramic material mainly comprises ceramic with low dielectric constant and low dielectric loss and an electromagnetic wave absorbent with high dielectric loss. The structural wave-absorbing integrated material with the functions of absorbing and bearing electromagnetic waves has wide and important application prospect in the stealth field of advanced aerospace crafts, land armors and ships. However, the existing wave-absorbing ceramic material has the disadvantages of low toughness, narrow effective absorption frequency band and the like, and is difficult to meet the use requirements in the application environment.
Document 1"Zhou W, et al, mechanical and Microwave-Absorption Properties of Si3N4 Ceramic with SiCNFs Fillers [ J]Advanced Engineering Materials,2018, "discloses the incorporation of SiC nanofibers (SiCNFs) into Si 3 N 4 A method in ceramics. The results show that with Si 3 N 4 The filling amount of SiCNFs in the matrix is increased, and the toughness of the material is controlled to be 3.4 MPa.m 1/2 Increased to 5.2 MPa.m 1/2 . In addition, in Si 3 N 4 SiCNFs filler is introduced into the ceramic, so that the complex dielectric constant and the dielectric loss can be obviously improved. But the toughness of the material is still low, and the broadband absorption of electromagnetic waves is not realized.
Document 2 Qi, et al, optimization of electronic Materials for Microwave Absorption [ J ]. Journal of Magnetic & Magnetic Materials,2011,323 (5): 600-606. "discloses a method of adjusting the dielectric and Magnetic properties of a material by varying the weight ratio of BaTiO3 and Carbonyl Iron (CI) particles. The results show that the material has a reflection loss of less than-10 dB in the frequency range of 10.8 to 14.8GHz, and a minimum reflection loss of-59 dB at a frequency of 12.5 GHz. But the material cannot achieve broadband absorption in the frequency range of 8 to 18GHz or more.
Therefore, the skilled in the art needs to provide a preparation method of a super-layered bionic ceramic with high toughness and capable of absorbing electromagnetic waves in a wide frequency, and the prepared super-layered bionic ceramic can improve the toughness and the electromagnetic wave absorption performance of a ceramic material at the same time, so that the super-layered bionic ceramic has a wide application prospect in the field of structure and function integration, and is easy to realize industrial production.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides the preparation method of the super-layered bionic ceramic with high toughness and broadband electromagnetic wave absorption, and the prepared super-layered bionic ceramic can simultaneously improve the toughness and the electromagnetic wave absorption performance of a ceramic material, so that the super-layered bionic ceramic has a wide application prospect in the field of structure and function integration and is easy to realize industrial production.
In order to achieve the purpose, the invention provides a preparation method of a high-toughness broadband electromagnetic wave absorption super-layer structure bionic ceramic, which comprises the following steps:
s01, preparing a base layer casting sheet;
adopting a benzene and alcohol mixed solution as a solvent, and adding a dispersing agent into the solvent until the dispersing agent is completely dissolved; then respectively adding a sintering aid and the ceramic particles of the matrix layer, selectively adding an electromagnetic wave absorbent, respectively adding a binder and a plasticizer after ball milling is uniform, and then ball milling is uniform; removing bubbles in vacuum to obtain uniform matrix layer casting slurry; wherein the matrix layer ceramic particles are Si 3 N 4 、AlN、B 4 C、MgO、SiO 2 、Al 2 O 3 、ZrO 2 、HfO 2 、ZrSiO 4 Or HfSiO 4 One or more of the materials are composed of complex phase ceramic particles;
adjusting the gap of a scraper of a casting machine, controlling the casting speed to carry out casting molding, and drying to obtain a base layer casting sheet;
s02, preparing an interface layer casting sheet;
adopting a benzene and alcohol mixed solution as a solvent, and adding a dispersing agent into the solvent until the dispersing agent is completely dissolved; then respectively adding a sintering aid and interface layer ceramic particles, selectively adding an electromagnetic wave absorbent, respectively adding a binder and a plasticizer after ball milling is uniform, and then ball milling is uniform; removing bubbles in vacuum to obtain uniform interface layer casting slurry; wherein the ceramic particles at the interface layer are BN and Y 2 Si 2 O 7 、Y 2 SiO 5 Or one of carbon materials or complex phase ceramic particles composed of a plurality of materials; adding an electromagnetic wave absorbing agent into at least one of the substrate layer casting sheet and the interface layer casting sheet;
adjusting the clearance of a scraper of a casting machine, controlling the casting speed to carry out casting molding, and drying to obtain an interface layer casting sheet;
s03, preparing a super-layered bionic ceramic material;
alternately laminating the base layer casting sheet in the step S01 and the interface layer casting sheet in the step S02 at intervals according to the thickness ratio of (2-15) to 1, and performing interference pressure molding on the laminated materials and then removing glue; sintering the sample subjected to the binder removal at a high temperature to obtain a super-layered bionic ceramic material; the matrix layer casting sheet and the interface layer casting sheet in the super-layered bionic ceramic material are distributed in a gradient structure, a periodic change structure or a low-high-low sandwich structure according to the content of the electromagnetic wave absorbent.
Preferably, the electromagnetic wave absorbent in step S01 and step S02 is SiC micron powder, siC nano powder, siC whisker, siC fiber, graphite powder, carbon black powder, carbon nanotube, graphene, carbon fiber, tiC, taC, zrC, hfC, tiB 2 、ZrB 2 、HfB 2 One or more of TaN, hfN and ZrN materials.
Preferably, a predetermined amount of matrix layer ceramic particles is added to the interface layer ceramic particles in step S02 to adjust the interface bonding strength.
Preferably, the step S01 of preparing the base layer casting sheet specifically includes the steps of:
taking a mixed solution of 30-60% by weight of alcohols and benzenes as a solvent, wherein the volume ratio of the alcohols to the benzenes is 3; adding 1-5 wt% dispersant into solvent, stirring for 2-20 min to dissolve completely; then adding 1-10% by weight of sintering aid, 30-50% by weight of matrix layer ceramic particles and electromagnetic wave absorbent, ball milling for 2-12 h, adding 2-4% by weight of binder and 3-6% by weight of plasticizer, and ball milling for 6-12 h; removing bubbles in vacuum for 5-30 min to obtain uniform matrix layer casting slurry with proper viscosity;
adjusting the scraper gap of a casting machine to be 25-200 mu m, controlling the casting speed to be 1-10 cm/s for casting, naturally drying in a fume hood for 8-24 h to obtain a matrix layer casting sheet, cutting the matrix layer casting sheet into required size, and sealing and storing after being torn off from a casting film.
Preferably, in step S01, the weight fraction of the mixed solution of alcohols and benzenes is 30-60%, the alcohols is one of ethanol or isopropanol, the benzenes is one of toluene or xylene, and the volume ratio of the alcohols to the benzenes is (0.3-3): 1; the dispersant is triethyl phosphate, and the weight percentage of the dispersant is 1 to 5 percent; the weight fraction of the adhesive and the plasticizer is 5-10%, the adhesive is one of PVB, PVP and PVA, the plasticizer is glycerol and dioctyl phthalate, the weight fraction of the matrix layer ceramic particles and the electromagnetic wave absorbent is 30-50%, and the weight ratio of the matrix layer ceramic particles to the microwave absorbent is 20; the weight percentage of the sintering aid is 1-10%.
Preferably, the step S02 of preparing the interfacial layer cast sheet specifically includes:
taking a mixed solution of 30-60% by weight of alcohols and benzenes as a solvent, wherein the volume ratio of the alcohols to the benzenes is (3); adding 1-5 wt% dispersant into solvent, stirring for 2-20 min to dissolve completely; then adding 1-10% of sintering aid by weight, 30-50% of interface layer ceramic particles by weight and an electromagnetic wave absorber by weight, ball-milling for 2-12 h, adding 2-4% of binder by weight and 3-6% of plasticizer by weight, and ball-milling for 6-12 h; removing bubbles in vacuum for 5-30 min to obtain uniform interface layer casting slurry with proper viscosity;
adjusting the scraper gap of a casting machine to be 25-200 mu m, controlling the casting speed to be 1-10 cm/s for casting, naturally drying in a fume hood for 8-24 h to obtain an interface layer casting sheet, cutting the interface layer casting sheet into required size, tearing off the interface layer casting sheet from a casting film, and sealing and storing.
Preferably, in step S02, the weight fraction of the mixed solution of alcohols and benzenes is 30 to 60%, the alcohols is one of ethanol or isopropanol, the benzenes is one of toluene or xylene, and the volume ratio of the alcohols to the benzenes is (0.3 to 3): 1; the dispersant is triethyl phosphate, and the weight percentage of the dispersant is 1 to 5 percent; the weight fraction of the adhesive and the plasticizer is 5-10%, the adhesive is one of PVB, PVP and PVA, the plasticizer is glycerol and dioctyl phthalate, the weight fraction of the interface layer ceramic particles and the electromagnetic wave absorbent is 30-50%, and the weight ratio of the interface layer ceramic particles to the microwave absorbent is 50; the weight percentage of the sintering aid is 1-10%.
Preferably, the super-layer bionic ceramic material is formed by alternately laminating the base layer casting sheet in the step S01 and the interface layer casting sheet in the step S02, wherein the lamination thickness is 2-30 mm.
Preferably, the laminated materials are subjected to interference press molding and then are subjected to gel discharging for 2 to 5 hours at the temperature of between 600 and 900 ℃; and (3) sintering the sample subjected to the binder removal at 1600-2000 ℃ under 1-30 MPa in an inert atmosphere for 0.5-6 h to obtain the super-layered bionic ceramic material.
The invention has the technical effects and advantages that:
1. alternately laminating a substrate layer casting sheet and an interface layer casting sheet, and preparing the super-layer bionic ceramic material by cutting, laminating, binder removal, high-temperature sintering and other processes; by controlling the content and distribution of the electromagnetic wave absorbent in the substrate layer and the interface layer, the super-layered bionic ceramic with the characteristics of low-high-low sandwich structure, namely impedance/loss gradient gradual change, impedance/loss periodic change or loss, is designed and prepared.
2. The introduction of weak interface can effectively improve the toughness of the ceramic material, and the toughness can exceed that of the ceramic material15MP·m 1/2 (ii) a Meanwhile, the broadband wave absorbing performance of the super-layer structure bionic ceramic material can be obtained by optimizing the content and distribution of the electromagnetic wave absorbent, the reflectivity is less than-10 dB in the range of 8-18GHz or a wider frequency range, and the prepared ceramic material can be widely applied to advanced stealth equipment;
3. the method has the advantages of easily obtained raw materials, simple process and equipment, strong designability and easy realization of industrial production, and the prepared sample has strong electromagnetic wave absorption capacity and high toughness and can meet the requirements of application environments.
Description of the figures
FIG. 1 is a process for preparing a super-layered bionic ceramic material according to the present invention;
FIG. 2 is a schematic representation of a substrate layer cast sheet and an interfacial layer cast sheet of the present invention after lamination;
FIG. 3 is a schematic diagram of a super-layered bionic ceramic material after binder removal and sintering in the invention;
FIG. 4 is a schematic view of a super-layered bionic ceramic material with a gradient structure according to the present invention;
FIG. 5 is a schematic view of a super-layered bionic ceramic material with a sandwich structure according to the present invention;
FIG. 6 is a schematic view of a super-layered bionic ceramic material with a periodically varying structure according to the present invention;
FIG. 7 is a graph of the reflection loss of the optimized material in example 1 of the present invention;
FIG. 8 is a graph of parallel ductile displacement loads for example 1 of the present invention;
FIG. 9 is a graph of vertical ductile displacement load for example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of a high-toughness broadband electromagnetic wave absorption super-layered bionic ceramic, which comprises the following steps of: s01, preparing a base layer casting sheet; s02, preparing an interface layer casting sheet; and S03, preparing the super-layered bionic ceramic material. The invention prepares the super-layer bionic ceramic material by alternately laminating the base layer casting sheet and the interface layer casting sheet, and then preparing the super-layer bionic ceramic material by processes of cutting, laminating, glue discharging, high-temperature sintering and the like.
In the step S01, preparing a matrix layer casting sheet, firstly, adopting a benzene and alcohol mixed solution as a solvent, and adding a dispersing agent into the solvent until the dispersing agent is completely dissolved; then respectively adding a sintering aid, matrix layer ceramic particles and an electromagnetic wave absorbing agent, respectively adding a binder and a plasticizer after ball milling is uniform, and then ball milling is uniform; obtaining uniform matrix layer casting slurry after vacuum bubble removal; and finally, adjusting the clearance of a scraper of the casting machine, controlling the casting speed to carry out casting molding, and drying to obtain the matrix layer casting sheet.
Wherein the matrix layer ceramic particles are Si 3 N 4 、AlN、B 4 C、MgO、SiO 2 、Al 2 O 3 、ZrO 2 、HfO 2 、ZrSiO 4 Or HfSiO 4 One or more of the materials are composed of complex phase ceramic particles; the electromagnetic wave absorbent is SiC micron powder, siC nanometer powder, siC crystal whisker, siC fiber, graphite powder, carbon black powder, carbon nano tube, graphene, carbon fiber, tiC, taC, zrC, hfC and TiB 2 、ZrB 2 、HfB 2 One or more of TaN, hfN and ZrN materials.
The benzene and alcohol are preferably ethanol and xylene or isopropanol and toluene; the dispersant is preferably triethyl phosphate; the sintering aid is preferably 1 to 10 weight percent of Al 2 O 3 :Y 2 O 3 The mass ratio is 1 2 :AlF 3 1; the binder is preferably PVB, PVP or PVA; the plasticizer is preferably glycerol and dioctyl phthalate DOP, wherein the volume ratio of the glycerol to the dioctyl phthalate DOP is 3.
Specifically, the preparation of the matrix layer casting sheet specifically comprises the following steps: taking a mixed solution of 30-60% by weight of alcohols and benzenes as a solvent, wherein the volume ratio of the alcohols to the benzenes is (3); adding 1-5 wt% dispersant into solvent, stirring for 2-20 min to dissolve completely; then adding 1-10% by weight of sintering aid, 30-50% by weight of matrix layer ceramic particles and electromagnetic wave absorbent, ball milling for 2-12 h, adding 2-4% by weight of binder and 3-6% by weight of plasticizer, and ball milling for 6-12 h; removing bubbles in vacuum for 5-30 min to obtain uniform matrix layer casting slurry with proper viscosity; and finally, adjusting the gap of a scraper of the casting machine to be 25-200 mu m, controlling the casting speed to be 1-10 cm/s for casting, naturally drying in a fume hood for 8-24 h to obtain a matrix layer casting sheet, cutting the matrix layer casting sheet into required size, and sealing and storing after being torn off from the casting film.
Wherein, the mixed solution of alcohols and benzenes with the weight fraction of 30-60 percent is used as a solvent, wherein the volume ratio of the alcohols to the benzenes is 3; adding 1-5 wt% dispersant into solvent, stirring for 2-20 min to dissolve completely; then adding 1-10% by weight of sintering aid, 30-50% by weight of matrix layer ceramic particles and an electromagnetic wave absorber, ball-milling for 2-12 h, adding 2-4% by weight of binder and 3-6% by weight of plasticizer, and ball-milling for 6-12 h; and removing bubbles in vacuum for 5-30 min to obtain uniform matrix layer casting slurry with proper viscosity.
In the step S02, preparing the boundary layer casting sheet, firstly, adopting a benzene and alcohol mixed solution as a solvent, and adding a dispersing agent into the solvent until the dispersing agent is completely dissolved; then respectively adding a sintering aid, interface layer ceramic particles and an electromagnetic wave absorbent, respectively adding a binder and a plasticizer after ball milling is uniform, and then ball milling is uniform; obtaining uniform boundary layer casting slurry after vacuum bubble removal; and finally, adjusting the clearance of a scraper of the casting machine, controlling the casting speed to carry out casting molding, and drying to obtain the interface layer casting sheet.
Wherein the ceramic particles at the interface layer are BN and Y 2 Si 2 O 7 、Y 2 SiO 5 Or one of carbon materials or complex phase ceramic particles composed of a plurality of materials; the electromagnetic wave absorbent is SiC micron powder, siC nanometer powder, siC whisker, siC fiber, graphite powder, carbon black powder, carbon nanotube, graphene, carbon fiber, tiC, taC, zrC, hfC, tiB 2 、ZrB 2 、HfB 2 One or more of TaN, hfN and ZrN materials.
The benzenes and alcohols are preferably ethanol and xylene or isopropanol and toluene; the dispersant is preferably triethyl phosphate; the sintering aid is preferably 1 to 10 weight percent of Al 2 O 3 :Y 2 O 3 The mass ratio is 1 2 :AlF 3 1; the binder is preferably PVB, PVP or PVA; the plasticizer is preferably glycerol and dioctyl phthalate DOP, wherein the volume ratio of the glycerol to the dioctyl phthalate DOP is 3.
Specifically, the preparation of the interfacial layer casting sheet specifically comprises the following steps: taking a mixed solution of 30-60% by weight of alcohols and benzenes as a solvent, wherein the volume ratio of the alcohols to the benzenes is (3); adding 1-5 wt% dispersant into solvent, stirring for 2-20 min to dissolve completely; then adding 1-10% by weight of sintering aid, 30-50% by weight of interface layer ceramic particles and electromagnetic wave absorbent, ball milling for 2-12 h, adding 2-4% by weight of binder and 3-6% by weight of plasticizer, and ball milling for 6-12 h; removing bubbles in vacuum for 5-30 min to obtain uniform interface layer casting slurry with proper viscosity; adjusting the scraper gap of a casting machine to be 25-200 mu m, controlling the casting speed to be 1-10 cm/s for casting, naturally drying in a fume hood for 8-24 h to obtain an interface layer casting sheet, cutting the interface layer casting sheet into required size, tearing off the interface layer casting sheet from a casting film, and sealing and storing.
Wherein, the weight percentage of the mixed solution of alcohols and benzenes is 30-60%, the alcohols are one of ethanol or isopropanol, the benzenes are one of toluene or xylene, and the volume ratio of the alcohols to the benzenes is (0.3-3): 1; the dispersant is triethyl phosphate, and the weight percentage of the dispersant is 1 to 5 percent; the weight fraction of the adhesive and the plasticizer is 5-10%, the adhesive is one of PVB, PVP and PVA, the plasticizer is glycerol and dioctyl phthalate, the weight fraction of the interface layer ceramic particles and the electromagnetic wave absorbent is 30-50%, and the weight ratio of the interface layer ceramic particles to the microwave absorbent is 50; the weight percentage of the sintering aid is 1-10%.
S03, preparing a super-layered bionic ceramic material, namely, alternately laminating the base layer casting sheet in the step S01 and the interface layer casting sheet in the step S02 at intervals according to the thickness ratio of (2-15) to 1, wherein the lamination thickness is 2-30 mm, and removing glue after performing interference compression molding on the laminated materials; sintering the sample subjected to glue removal at high temperature to obtain a super-layered bionic ceramic material; the matrix layer casting sheet and the interface layer casting sheet in the super-layer bionic ceramic material are distributed in a gradient structure, a periodic change structure or a low-high-low sandwich structure according to the content of the electromagnetic wave absorbent.
Specifically, in the step, the laminated materials are subjected to interference press molding and then are subjected to gel discharging at the temperature of 600-900 ℃ for 2-5 h; and (3) sintering the sample subjected to the binder removal at 1600-2000 ℃ under 1-30 MPa in an inert atmosphere for 0.5-6 h to obtain the super-layered bionic ceramic material.
The invention prepares the super-layer bionic ceramic material by alternately laminating the substrate layer casting sheets and the interface layer casting sheets, and then preparing the super-layer bionic ceramic material by cutting, laminating, binder removal, high-temperature sintering and other processes; by controlling the content and distribution of the electromagnetic wave absorbent in the substrate layer and the interface layer, the super-layered bionic ceramic with the characteristics of low-high-low sandwich structure, namely impedance/loss gradient gradual change, impedance/loss periodic change or loss, is designed and prepared.
Example one
In step S01, si is prepared 3 N 4 -a SiC matrix layer cast sheet; taking 100g of matrix layer casting slurry as an example, taking 60g of ethanol and xylene as solvents, wherein the volume ratio of the ethanol to the xylene is 1; 2g of triethyl phosphate are added to the solvent, stirred for 20min and then 1.5g of Al are added 2 O 3 、1.5g Y 2 O 3 30g of SiC and Si 3 N 4 Wherein, in the step (A),the sintering auxiliary agent is Al 2 O 3 And Y 2 O 3 The electromagnetic wave absorbent SiC nano powder and the ceramic particles of the substrate layer are Si 3 N 4 (ii) a After ball milling for 5h (the rotating speed is 180 r/min), 2g of PVB as a binder, 1.5g of glycerol as a plasticizer and 1.5g of DOP are added, and then ball milling is carried out for 8h; and removing bubbles in vacuum for 15min to obtain uniform matrix layer casting slurry with proper viscosity. Wherein the electromagnetic wave absorbent SiC nano powder in the casting slurry of the substrate layer accounts for the total ceramic powder (Si) 3 N 4 And SiC nano powder) are 0%,30%,45%, respectively.
Adjusting the gap of a scraper of a casting machine to be 150 mu m, controlling the casting speed to be 5cm/s for casting, and naturally drying in a fume hood for 20 hours to obtain a matrix layer casting sheet; and cutting the casting sheet of the substrate layer into required size, and sealing and storing after being taken off from the casting film.
In step S02, preparing a BN interface layer tape-casting sheet; taking 100g of casting slurry as an example, taking 60g of ethanol and xylene as solvents, wherein the volume ratio of the ethanol to the xylene is 1; adding 2g triethyl phosphate into the solvent, stirring for 20min, then adding 1.5g Al 2 O 3 、1.5g Y 2 O 3 And 25g of BN, and ball milling for 5 hours (the rotating speed is 180 r/min); wherein the sintering aid is Al 2 O 3 And Y 2 O 3 The interface layer ceramic particles are BN; after ball milling, adding 2g of PVB as a binder, 1.5g of glycerol as a plasticizer and 1.5g of DOP, and then carrying out ball milling for 8 hours; and removing bubbles in vacuum for 15min to obtain uniform interface layer casting slurry with proper viscosity.
The thickness of a scraper of the casting machine is adjusted to be 50 mu m, and the casting speed is controlled to be 5cm/s for casting. Naturally drying in a fume hood for 20h to obtain an interface layer casting sheet; and cutting the boundary layer casting sheet into a required size, and sealing and storing after the boundary layer casting sheet is peeled off from the casting film.
In step S03, si is prepared 3 N 4 -SiC/BN biomimetic ceramic material: si in step S01 3 N 4 Alternately laminating the-SiC matrix layer casting sheets and the BN interface layer casting sheets in the step S02 at intervals, wherein the matrix layer casting sheets are sequentially laminated from bottom to top in an increasing mode of the content of the SiC nano powder of the electromagnetic wave absorbent, and the thickness of the laminated layers is divided into10mm for the cast sheet containing 0-percent SiC, 7mm for the cast sheet containing 30-percent SiC and 3mm for the cast sheet containing 45-percent SiC, respectively; pre-pressing the laminated sample, and then carrying out gel discharging for 2h at 800 ℃; the sample after the rubber removal is at 1850 ℃, the pressure is 30MPa, and the atmosphere is N 2 Hot pressed sintering for 1h to obtain Si 3 N 4 -SiC/BN super-layered bionic ceramic material.
Referring to figures 7-9 of the drawings, FIG. 7 is a graph of the reflection loss of the optimized material in example 1 of the present invention; FIG. 8 is a graph of parallel ductile displacement loads for example 1 of the present invention; FIG. 9 is a graph of vertical ductile displacement load for example 1 of the present invention. FIG. 7 with Si 3 N 4 the-SiC is used as a matrix layer, the BN is an RL curve of a double-layer wave-absorbing material consisting of interface layers, wherein the reflection coefficients of the optimized material are all less than-10 dB in the range of 8-18GHZ, and two resonance absorption peaks appear at 8.9GHz and 15.6GHz respectively. FIG. 8 is Si 3 N 4 And (3) a load displacement curve of a single-edge notched beam test of the SiC/BN laminated ceramic sample, wherein the load direction is parallel to the lamination direction, and the maximum load is 130.3N. The yield-phase curve is jagged with the maximum load not appearing at the first peak and the layered ceramic failing without exhibiting sudden fracture of the monolithic ceramic material, whereas the vertical ductile displacement load of fig. 9 exhibits sudden fracture.
Referring to Table 1, table 1 shows Si in example 1 of the present invention 3 N 4 -mechanical property data of the SiC/BN biomimetic ceramic material;
Figure BDA0003726212660000111
example two
In step S01, si is prepared 3 N 4 Casting a sheet on the substrate layer; taking 100g of casting slurry as an example, taking 60g of ethanol and xylene as solvents, wherein the volume ratio of the ethanol to the xylene is 1; adding 2g triethyl phosphate into the solvent, stirring for 20min, then adding 1.5g Al 2 O 3 、1.5g Y 2 O 3 、30g Si 3 N 4 Wherein the sintering aid is Al 2 O 3 And Y 2 O 3 The ceramic particles of the matrix layer being Si 3 N 4 (ii) a Ball milling for 5h (the rotating speed is 180 r/min), adding 2g of adhesive PVB, 2g of plasticizer glycerol and 1g of DOP, and then ball milling for 8h; and removing bubbles in vacuum for 15min to obtain uniform casting slurry with proper viscosity.
Adjusting the scraper gap of a casting machine to be 150 mu m, controlling the casting speed to be 5cm/s for casting, and naturally drying in a fume hood for 20h to obtain a matrix layer casting sheet; the cast sheet is cut to a desired size, and is sealed and stored after being peeled off from the cast film.
In step S02, preparing a SiC-BN interface layer casting sheet, taking 100g of casting slurry as an example, taking 60g of ethanol and xylene as solvents, wherein the volume ratio of ethanol to xylene is 1; adding 2g triethyl phosphate into the solvent, stirring for 20min, then adding 1.5g Al 2 O 3 、1.5g Y 2 O 3 30g of SiC fiber and BN powder, wherein the sintering aid is Al 2 O 3 And Y 2 O 3 The electromagnetic wave absorbent is SiC fiber, and the interface layer ceramic particles are BN; after ball milling for 5h (the rotating speed is 180 r/min), 2g of adhesive PVB, 1.5g of plasticizer glycerol and 1.5g of DOP are added, and then ball milling is carried out for 8h; and removing bubbles in vacuum for 15min to obtain uniform casting slurry with proper viscosity. Wherein, the mass fractions of the electromagnetic wave absorbent SiC fibers in the boundary layer casting slurry in the total ceramic powder (BN and SiC fibers) are respectively 0%,30% and 45%.
The thickness of a scraper of the casting machine is adjusted to be 50 mu m, and the casting speed is controlled to be 5cm/s for casting. Naturally drying the mixture in a fume hood for 20 hours to obtain an interfacial layer casting sheet; the cast sheet is cut to a desired size, and is sealed and stored after being peeled off from the cast film.
In step S03, si is prepared 3 N 4 The SiC-BN bionic ceramic material is prepared by mixing Si in the step S01 3 N 4 Alternately laminating the substrate layer casting sheets and the SiC-BN interface layer casting sheets in the step S02 at intervals; wherein the boundary layer casting sheets were laminated in the manner that the content of the electromagnetic wave absorber SiC fibers was increased from bottom to top in this order, the thickness of the laminated boundary layer casting sheets each containing 0% of SiC fibers was 9mm, the content of the laminated boundary layer casting sheets each containing 30% of SiC fibers was 9mmSheet 6mm and interface layer cast sheet 3mm containing 45% SiC fibers; pre-pressing the laminated sample, and then carrying out gel discharging for 2h at 900 ℃; the sample after the rubber removal is at 1850 ℃, the pressure is 30MPa, and the atmosphere is N 2 Hot pressed sintering for 2h to obtain Si 3 N 4 the/SiC-BN super-layered bionic ceramic material.
EXAMPLE III
In step S01, preparing an AlN-CNT matrix layer casting sheet; taking 100g of casting slurry as an example, taking 60g of ethanol and xylene as solvents, wherein the volume ratio of the ethanol to the xylene is 1; adding 2g triethyl phosphate into the solvent, stirring for 20min, then adding 2g AlF 3 、1g MgF 2 30g of CNT and AlN, wherein the sintering aid is MgF 2 And AlF 3 The electromagnetic wave absorber is carbon nano tube CNT, and the ceramic particles of the substrate layer are AlN; ball milling is carried out for 5h (2 g of adhesive PVB, 2g of plasticizer glycerol and 1g of DOP are added after the rotating speed is 180r/min, ball milling is carried out for 8h, and vacuum bubble removal is carried out for 15min to obtain uniform matrix layer casting slurry with proper viscosity, wherein the mass fractions of the electromagnetic wave absorber CNT in the matrix layer casting slurry in the total ceramic powder (CNT and AlN) are respectively 1% and 5%.
Adjusting the scraper gap of a casting machine to be 150 mu m, controlling the casting speed to be 5cm/s for casting, and naturally drying in a fume hood for 20h to obtain a matrix layer casting sheet; and cutting the casting sheet of the substrate layer into required size, and sealing and storing after being taken off from the casting film.
In step S02, preparing an AlN-BN interface layer casting sheet, taking 100g of casting slurry as an example, taking 60g of ethanol and xylene as solvents, wherein the volume ratio of the ethanol to the xylene is 1; adding 2g triethyl phosphate into the solvent, stirring for 20min, then adding 2g AlF 3 、1g MgF 2 5g of AlN and 25g of BN; wherein the sintering aid is MgF 2 And AlF 3 The interfacial layer ceramic particles are BN and AlN; after ball milling for 5 hours (the rotating speed is 180 r/min), 2g of adhesive PVB, 2g of plasticizer glycerol and 1g of DOP are added, and then ball milling is carried out for 8 hours; and removing bubbles in vacuum for 15min to obtain uniform interfacial layer casting slurry with proper viscosity.
The thickness of a scraper of the casting machine is adjusted to be 25 mu m, and the casting speed is controlled to be 5cm/s for casting. Naturally drying in a fume hood for 20h to obtain an interface layer casting sheet; and cutting the boundary layer casting sheet into a required size, and sealing and storing after the boundary layer casting sheet is stripped from the casting film.
In step S03, preparing an AlN-CNT/BN bionic ceramic material; alternately laminating the AlN-CNT matrix layer casting sheet of the step S01 and the AlN-BN interfacial layer casting sheet of the step S02 at intervals, wherein the matrix layers are laminated in a sandwich structure of "low-high-low" in order from bottom to top, the lamination thickness is 6mm for the casting sheet containing 1% of CNT, 8mm for the casting sheet containing 5% of CNT and 6mm for the casting sheet containing 1% of CNT, respectively, and the laminated sample is subjected to dry compression molding and then discharged at 900 ℃ for 2h; the sample after the rubber removal is carried out at 1800 ℃, the pressure is 30MPa, and the atmosphere is N 2 And hot-pressing and sintering for 2h to obtain the AlN-CNT/BN super-layered bionic ceramic material.
Example four
In step S01, preparing a MgO-graphite powder (C) matrix layer casting sheet, taking 100g of casting slurry as an example, taking 60g of ethanol and xylene as solvents, wherein the volume ratio of ethanol to xylene is 1; adding 2g triethyl phosphate into the solvent, stirring for 20min, then adding 1g AlF 3 、2g MgF 2 20g of C and MgO powder, wherein the sintering aid is MgF 2 And AlF 3 The electromagnetic wave absorbent is C, and the ceramic particles of the matrix layer are MgO; after ball milling is carried out for 3h (the rotating speed is 180 r/min), 2g of adhesive PVB, 2g of plasticizer glycerol and 1g of DOP are added, and then ball milling is carried out for 5h; and removing bubbles in vacuum for 20min to obtain uniform matrix layer casting slurry with proper viscosity. Wherein, the mass fractions of the electromagnetic wave absorbent graphite powder in the total ceramic powder (MgO and C) in the matrix layer casting slurry are respectively 10%,30% and 50%.
Adjusting the scraper gap of a casting machine to be 150 mu m, controlling the casting speed to be 2cm/s for casting, and naturally drying in a fume hood for 20h to obtain a matrix layer casting sheet; and cutting the casting sheet of the substrate layer into a required size, and sealing and storing after being taken off from the casting film.
In step S02, an MgO-BN interfacial layer casting sheet is prepared, taking 100g of casting slurry as an example, and taking 60g of ethanol and xylene as solvents, wherein the volume ratio of the ethanol to the xylene is 11, preparing a catalyst; adding 2g triethyl phosphate into the solvent, stirring for 20min, then adding 1g AlF 3 、2g MgF 2 5g of MgO and 25g of BN, wherein the sintering aid is MgF 2 And AlF 3 The interface layer ceramic particles are BN, and the matrix layer ceramic particles MgO are additionally added to adjust the interface bonding strength; after ball milling is carried out for 3h (the rotating speed is 180 r/min), 2g of adhesive PVB, 2g of plasticizer glycerol and 1g of DOP are added, and then ball milling is carried out for 5h; and removing bubbles in vacuum for 15min to obtain uniform interfacial layer casting slurry with proper viscosity.
The thickness of a scraper of the casting machine is adjusted to be 25 mu m, and the casting is carried out by controlling the casting speed to be 2 cm/s. Naturally drying in a fume hood for 20h to obtain an interface layer casting sheet; and cutting the boundary layer casting sheet into a required size, and sealing and storing after the boundary layer casting sheet is peeled off from the casting film.
In step S03, preparing a MgO-SiC/BN biomimetic ceramic material, alternately laminating the MgO-C matrix layer casting sheets in step S01 and the MgO-BN interface layer casting sheets in step S02 at intervals, wherein the matrix layer casting sheets are sequentially laminated from bottom to top in an increasing manner of the content of the electromagnetic wave absorbing agent C, the lamination thicknesses are respectively 9mm for the casting sheet containing 10% C, 7mm for the casting sheet containing 30% C and 4mm for the casting sheet containing 50% SiC, and the laminated sample is subjected to dry compaction molding and is then discharged for 5h at 900 ℃; the sample after the rubber removal is at 1650 ℃, the pressure is 30MPa, and the atmosphere is N 2 And carrying out hot-pressing sintering for 2h to obtain the MgO-C/BN super-layered bionic ceramic material.
EXAMPLE five
In step S01, si is prepared 3 N 4 -SiC matrix layer cast sheet, taking 100g of cast slurry as an example, taking 60g of ethanol and xylene as solvents, wherein the volume ratio of ethanol to xylene is 1; adding 2g triethyl phosphate into the solvent, stirring for 20min, then adding 0.5g Al 2 O 3 、2.5g Y 2 O 3 30g of SiC whisker and Si 3 N 4 Powder, wherein the sintering aid is Al 2 O 3 And Y 2 O 3 The electromagnetic wave absorber is SiC crystal whisker, and the ceramic particles of the substrate layer are Si 3 N 4 (ii) a After ball milling for 5h (rotating speed 180 r/min), 2g of adhesive PVB, 1.5g of plasticizer glycerol and 1 are added.5g DOP, and then ball milling is carried out for 5 hours; and removing bubbles in vacuum for 20min to obtain uniform matrix layer casting slurry with proper viscosity. Wherein the SiC whiskers as the electromagnetic wave absorbent in the casting slurry of the substrate layer account for the total ceramic powder (Si) 3 N 4 And SiC whiskers) were 10%,45%, respectively.
Adjusting the gap of a scraper of a casting machine to be 150 mu m, controlling the casting speed to be 5cm/s for casting, and naturally drying in a fume hood for 20 hours to obtain a matrix layer casting sheet; and cutting the casting sheet of the substrate layer into a required size, and sealing and storing after being taken off from the casting film.
In step S02, si is prepared 3 N 4 -Y 2 Si 2 O 7 Taking 100g of casting slurry as an example, taking 60g of ethanol and xylene as solvents, wherein the volume ratio of the ethanol to the xylene is 1; adding 2g triethyl phosphate into the solvent, stirring for 20min, then adding 0.5g Al 2 O 3 、2.5g Y 2 O 3 、5g Si 3 N 4 And 25g of Y 2 Si 2 O 7 Wherein the sintering aid is Al 2 O 3 And Y 2 O 3 The interfacial layer ceramic particles are Y 2 Si 2 O 7 (ii) a Additionally adding matrix layer ceramic particles Si 3 N 4 To adjust the interface bonding strength; after ball milling for 5h (the rotating speed is 180 r/min), 2g of adhesive PVB, 1.5g of plasticizer glycerol and 1.5g of DOP are added, and then ball milling is carried out for 5h; and removing bubbles in vacuum for 20min to obtain uniform interface layer casting slurry with proper viscosity.
The thickness of a scraper of the casting machine is adjusted to be 50 mu m, and the casting speed is controlled to be 5cm/s for casting. Naturally drying in a fume hood for 20h to obtain an interface layer casting sheet; and cutting the boundary layer casting sheet into a required size, and sealing and storing after the boundary layer casting sheet is stripped from the casting film.
In step S03, si is prepared 3 N 4 -SiC/Y 2 Si 2 O 7 A biomimetic ceramic material; si in step S01 3 N 4 Cast sheet of-SiC base layer and Si in step S02 3 N 4 -Y 2 Si 2 O 7 Alternately stacked at intervals of boundary layer cast sheets, wherein the substrateLaminating the laminated cast sheets in the mode of periodically changing the content of the electromagnetic wave absorbing agent SiC from bottom to top, wherein the lamination thickness is respectively 3mm of the cast sheet containing 10-percent SiC whiskers, 7mm of the cast sheet containing 45-percent SiC, 3mm of the cast sheet containing 10-percent SiC and 7mm of the cast sheet containing 45-percent SiC whiskers, and the laminated sample is subjected to interference press molding and then is subjected to gel discharging at 800 ℃ for 3h; the sample after the rubber removal is carried out at 1700 ℃, the pressure is 30MPa and the atmosphere is N 2 Hot pressed sintering for 2h to obtain Si 3 N 4 -SiC/Y 2 Si 2 O 7 The super-layered bionic ceramic material.
Finally, the above description is only for the preferred embodiment of the present invention and should not be taken as limiting the invention, and any modifications, equivalents, improvements and the like which are within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (9)

1. A preparation method of a high-toughness broadband electromagnetic wave absorbing super-layer structure bionic ceramic is characterized by comprising the following steps:
s01, preparing a base layer casting sheet;
adopting a benzene and alcohol mixed solution as a solvent, and adding a dispersing agent into the solvent until the dispersing agent is completely dissolved; then respectively adding a sintering aid and the ceramic particles of the matrix layer, selectively adding an electromagnetic wave absorbent, respectively adding a binder and a plasticizer after ball milling is uniform, and then ball milling is uniform; removing bubbles in vacuum to obtain uniform matrix layer casting slurry; wherein the matrix layer ceramic particles are Si 3 N 4 、AlN、B 4 C、MgO、SiO 2 、Al 2 O 3 、ZrO 2 、HfO 2 、ZrSiO 4 Or HfSiO 4 One or more of the materials are composed of complex phase ceramic particles;
adjusting the clearance of a scraper of a casting machine, controlling the casting speed to carry out casting molding, and drying to obtain a base layer casting sheet;
s02, preparing an interface layer casting sheet;
adopting benzene and alcohol mixed liquor as solvent, adding dispersing agent into the solventCompletely dissolving; then respectively adding a sintering aid and interface layer ceramic particles, selectively adding an electromagnetic wave absorbent, respectively adding a binder and a plasticizer after ball milling is uniform, and then ball milling is uniform; obtaining uniform boundary layer casting slurry after vacuum bubble removal; wherein the ceramic particles at the interface layer are BN, Y 2 Si 2 O 7 、Y 2 SiO 5 Or one of the carbon materials or complex phase ceramic particles consisting of a plurality of the materials; adding an electromagnetic wave absorbent into at least one of the base layer casting sheet and the interface layer casting sheet;
adjusting the clearance of a scraper of a casting machine, controlling the casting speed to carry out casting molding, and drying to obtain an interface layer casting sheet;
s03, preparing a super-layered bionic ceramic material;
alternately laminating the base layer casting sheet in the step S01 and the interface layer casting sheet in the step S02 at intervals according to the thickness ratio of (2-15) to 1, and performing interference pressure molding on the laminated materials and then removing glue; sintering the sample subjected to the binder removal at a high temperature to obtain a super-layered bionic ceramic material; the matrix layer casting sheet and the interface layer casting sheet in the super-layered bionic ceramic material are distributed in a gradient structure, a periodic change structure or a low-high-low sandwich structure according to the content of the electromagnetic wave absorbent.
2. The method for preparing a high-toughness broadband electromagnetic wave absorbing super-layered bionic ceramic according to claim 1, wherein the electromagnetic wave absorber in the steps S01 and S02 is SiC micron powder, siC nano powder, siC whisker, siC fiber, graphite powder, carbon black powder, carbon nanotube, graphene, carbon fiber, tiC, taC, zrC, hfC, tiB 2 、ZrB 2 、HfB 2 One or more of TaN, hfN and ZrN materials.
3. The method for preparing a high-toughness broadband electromagnetic wave absorbing multilayer bionic ceramic according to claim 1, wherein a preset amount of matrix layer ceramic particles are added to the interface layer ceramic particles in step S02 to adjust the interface bonding strength.
4. The method for preparing the multilayer bionic ceramic with high toughness and broadband electromagnetic wave absorption according to claim 1, wherein the step S01 of preparing the base layer casting sheet specifically comprises the following steps:
taking a mixed solution of 30-60% by weight of alcohols and benzene as a solvent, wherein the volume ratio of the alcohols to the benzene is 3; adding 1-5 wt% of dispersant into the solvent, and stirring for 2-20min until the dispersant is completely dissolved; then adding 1-10% by weight of a sintering aid, 30-50% by weight of matrix layer ceramic particles and an electromagnetic wave absorber, ball-milling for 2-12h, adding 2-4% by weight of a binder and 3-6% by weight of a plasticizer, and ball-milling for 6-12h; removing bubbles in vacuum for 5 to 30min to obtain uniform matrix layer casting slurry with proper viscosity;
and adjusting the gap of a scraper of the casting machine to be 25-200 mu m, controlling the casting speed to be 1-10cm/s, carrying out casting, naturally drying in a fume hood for 8-24h to obtain a base layer casting sheet, cutting the base layer casting sheet into a required size, tearing off the base layer casting sheet from the casting film, and sealing and storing.
5. The method for preparing the multilayer bionic ceramic with high toughness and broadband electromagnetic wave absorption according to claim 1, wherein in step S01, the weight fraction of a mixed solution of alcohol and benzene is 30-60%, the alcohol is one of ethanol or isopropanol, the benzene is one of toluene or xylene, and the volume ratio of the alcohol to the benzene is (0.3-3): 1; the dispersant is triethyl phosphate, and the weight percentage of the dispersant is 1 to 5 percent; the weight percentage of the binder and the plasticizer is 5 to 10 percent, the binder is one of PVB, PVP and PVA, the plasticizer is glycerol and dioctyl phthalate, the weight percentage of the matrix layer ceramic particles and the electromagnetic wave absorbent is 30 to 50 percent, and the weight ratio of the matrix layer ceramic particles to the electromagnetic wave absorbent is 20 to 1; the weight fraction of the sintering aid is 1 to 10 percent.
6. The method for preparing a high-toughness broadband electromagnetic wave absorbing super-layered bionic ceramic according to claim 1, wherein the step S02 of preparing the interface layer casting sheet specifically comprises:
taking a mixed solution of 30-60% by weight of alcohols and benzene as a solvent, wherein the volume ratio of the alcohols to the benzene is 3; adding a dispersing agent with the weight percentage of 1 to 5 percent into a solvent, and stirring for 2 to 20min until the dispersing agent is completely dissolved; then adding 1-10% by weight of a sintering aid, 30-50% by weight of interface layer ceramic particles and an electromagnetic wave absorbent, ball-milling for 2-12h, adding 2-4% by weight of a binder and 3-6% by weight of a plasticizer, and ball-milling for 6-12h; removing bubbles in vacuum for 5 to 30min to obtain uniform interface layer casting slurry with proper viscosity;
and adjusting the gap of a scraper of the casting machine to be 25-200 mu m, controlling the casting speed to be 1-10cm/s, carrying out casting, naturally drying in a fume hood for 8-24h to obtain an interface layer casting sheet, cutting the interface layer casting sheet into a required size, tearing off the interface layer casting sheet from the casting film, and sealing and storing.
7. The method for preparing the multilayer bionic ceramic with high toughness and broadband electromagnetic wave absorption according to claim 1, wherein in step S02, the weight fraction of the mixed solution of alcohols and benzenes is 30-60%, the alcohols is one of ethanol or isopropanol, the benzenes is one of toluene or xylene, and the volume ratio of the alcohols to the benzenes is (0.3-3): 1; the dispersant is triethyl phosphate, and the weight percentage of the dispersant is 1 to 5 percent; the weight fraction of the binder and the plasticizer is 5-10%, the binder is one of PVB, PVP and PVA, the plasticizer is glycerol and dioctyl phthalate, the weight fraction of the interface layer ceramic particles and the electromagnetic wave absorbent is 30-50%, and the weight ratio of the interface layer ceramic particles to the electromagnetic wave absorbent is 50; the weight fraction of the sintering aid is 1-10%.
8. The method for preparing the super-layered bionic ceramic with high toughness and broadband electromagnetic wave absorption according to claim 1, wherein the super-layered bionic ceramic material is prepared by alternately laminating the base layer casting sheet in the step S01 and the interface layer casting sheet in the step S02, wherein the lamination thickness is 2-30mm.
9. The preparation method of the high-toughness broadband electromagnetic wave absorption super-layered bionic ceramic according to claim 8, wherein the laminated materials are subjected to interference press molding and then are subjected to glue discharging at 600-900 ℃ for 2-5 h; and (3) sintering the sample after the glue discharging at 1600-2000 ℃ and 1-30MPa for 0.5-6 h in an inert atmosphere to obtain the super-laminar bionic ceramic material.
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