CN117467238A - High-temperature-resistant high-heat-conductivity rigid wave-absorbing material and preparation method thereof - Google Patents
High-temperature-resistant high-heat-conductivity rigid wave-absorbing material and preparation method thereof Download PDFInfo
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- 239000011358 absorbing material Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 65
- 229910000599 Cr alloy Inorganic materials 0.000 claims abstract description 40
- 239000000788 chromium alloy Substances 0.000 claims abstract description 40
- 229910000519 Ferrosilicon Inorganic materials 0.000 claims abstract description 38
- 238000005245 sintering Methods 0.000 claims abstract description 34
- 229910052582 BN Inorganic materials 0.000 claims abstract description 24
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 23
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 23
- 239000005011 phenolic resin Substances 0.000 claims abstract description 23
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000011812 mixed powder Substances 0.000 claims abstract description 21
- -1 propargyl phenolic resin Chemical compound 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 11
- 238000000498 ball milling Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 17
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 16
- 239000004327 boric acid Substances 0.000 claims description 16
- 229910045601 alloy Inorganic materials 0.000 claims description 12
- 239000000956 alloy Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 5
- 229910008458 Si—Cr Inorganic materials 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 15
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 11
- 238000000576 coating method Methods 0.000 description 10
- 239000011248 coating agent Substances 0.000 description 9
- 238000000465 moulding Methods 0.000 description 7
- 239000011230 binding agent Substances 0.000 description 5
- 230000009477 glass transition Effects 0.000 description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 238000005253 cladding Methods 0.000 description 4
- 239000011247 coating layer Substances 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 3
- XEVZIAVUCQDJFL-UHFFFAOYSA-N [Cr].[Fe].[Si] Chemical compound [Cr].[Fe].[Si] XEVZIAVUCQDJFL-UHFFFAOYSA-N 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- XQUPVDVFXZDTLT-UHFFFAOYSA-N 1-[4-[[4-(2,5-dioxopyrrol-1-yl)phenyl]methyl]phenyl]pyrrole-2,5-dione Chemical group O=C1C=CC(=O)N1C(C=C1)=CC=C1CC1=CC=C(N2C(C=CC2=O)=O)C=C1 XQUPVDVFXZDTLT-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 239000006057 Non-nutritive feed additive Substances 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000012224 working solution Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses a high-temperature-resistant high-heat-conductivity rigid wave-absorbing material and a preparation method thereof, and relates to the field of electromagnetic wave-absorbing materials; placing the ball-milled mixed powder into a high-temperature sintering furnace, and sintering in an ammonia atmosphere to obtain boron nitride coated ferrosilicon chromium alloy powder; and uniformly mixing the obtained coated ferrosilicon chromium alloy powder with propargyl phenolic resin, and curing and forming the mixture in a mold to obtain the high-temperature-resistant high-heat-conductivity rigid wave-absorbing material. The high-temperature-resistant high-heat-conductivity wave-absorbing material has excellent high-temperature resistance, heat-conducting performance and microwave absorption performance.
Description
Technical Field
The invention relates to the field of electromagnetic wave absorbing materials, in particular to a high-temperature-resistant high-heat-conductivity rigid wave absorbing material and a preparation method thereof.
Background
The rigid wave-absorbing material is mainly composed of an absorbent, a binder and various processing aids, is a multifunctional polymer composite material, has wave-absorbing performance of electromagnetic interference resistance, microwave orientation enhancement and clutter suppression, and also has multiple performances of high and low temperature resistance, bearing capacity and the like, and is mainly applied to electronic devices such as antennas, microwave components, synthetic splitters, isolators, feed networks and the like of aerospace equipment.
When the rigid wave absorbing material is used for antenna and microwave components, the rigid wave absorbing material has the main functions of absorbing clutter and the like, and also needs to meet the requirements of high temperature resistance and high heat conductivity under high temperature conditions. Taking the use requirement of a wave-absorbing material in a new generation of aircraft as an example, as the antenna works in a high-power active receiving-transmitting array mode, the internal working temperature can reach about 250 ℃ due to the absorption of the power loss of an antenna port, and the wave-absorbing material is required to withstand long-time high-temperature working conditions and not to fail; in addition, the antenna unit or the welding spot can be damaged due to long-term high temperature, the antenna performance is seriously affected, and the heat generated in the antenna unit or the welding spot needs to be dissipated in time to reduce the temperature of the antenna. Therefore, the wave-absorbing material used in the antenna is required to have good heat conduction and heat dissipation performance (the heat conduction coefficient is more than or equal to 2W/(m & ltK+ & gt) (under the room temperature condition), and the heat conduction coefficient of the conventional wave-absorbing material is 1.1W/(m & ltK) (under the room temperature condition), so that the use requirements of the antenna are greatly different from those of the model.
At present, a commonly used high-performance absorber of the wave-absorbing material is carbonyl iron powder, the absorption performance of the powder is fast attenuated at a long-term high temperature, the powder is not suitable for a high-temperature working condition, and aiming at the problem of low heat conduction performance of the wave-absorbing material, the conventional method for improving the heat conduction performance of the material is to mechanically mix heat conduction fillers (aluminum oxide, magnesium oxide, zinc oxide, aluminum nitride, boron nitride, silicon carbide and the like) into slurry, but the conventional metal oxide heat conduction fillers influence the wave-absorbing performance of the material and are not suitable for addition; and the fillers such as boron nitride, silicon carbide and the like are difficult to form a continuous and efficient heat conduction network in a mechanical mixing and adding mode, so that the heat conduction performance of the obtained wave-absorbing material is improved slightly.
In addition, in the prior art, iron-silicon-chromium powder is used as a raw material for preparation, for example, patent CN109326405a discloses a preparation method of high-heat-conductivity insulating soft magnetic metal powder and soft magnetic metal powder, wherein the surface of the iron-silicon-chromium powder is coated mainly by a chemical deposition method, and then mixed and granulated by adopting epoxy, phenolic resin and other resins to prepare the soft magnetic metal powder; the powder is coated by a chemical mode, and the temperature resistance of the epoxy resin and the phenolic resin used is not more than 250 ℃. The patent CN111234777A is mainly characterized in that the surface of the ferrosilicon chromium powder is coated in a chemical and physical combination mode, an aminosilane coupling agent coating layer is firstly formed on the surface of the ferrosilicon chromium powder, and then boric acid and orthosilicic acid in the working solution are mixed with the boric acid and the orthosilicic acid through ball milling to form a boric acid and orthosilicic acid coating layer through hydrogen bonding; the used adhesive is a water-based adhesive, and is required to be catalytically cured by a curing agent; the prepared product is the coated laminate wave-absorbing material. The patent CN115365488A adopts ferrosilicon chromium powder to prepare the wave-absorbing material, but the powder is not modified, the prepared wave-absorbing material does not have high heat conduction performance, and the adhesive is modified bismaleimide resin. The patent CN116102791A is mainly characterized in that the surface of the ferrosilicon chromium powder is coated in a chemical and physical combined mode, the principle is slightly different from that of the patent CN111234777A, a layer of sulfhydryl silane coupling agent coating layer is firstly formed on the surface of the ferrosilicon chromium powder, then the surface of the ferrosilicon chromium powder is mixed with boron nitride in a ball milling mode to form a boron nitride coating layer through the action of B-H bonds, the used binder is silicon rubber, and the prepared wave absorbing material is a flexible material. The patent CN116156858A is to coat the surface of the ferrosilicon chromium powder by zinc oxide, so as to obtain modified powder, and prepare the high-wave-absorbing material by using the powder, wherein the used binder is polyurethane, and the temperature resistance is lower. Patent CN116179118A discloses a method for preparing a heat absorbing and conducting material, a tape, an electronic component and a tape, which adopts ferrosilicon chromium powder and boron nitride to prepare the heat absorbing and conducting tape by doping in a simple physical mixing mode.
Therefore, in order to overcome the above disadvantages, it is necessary to provide a rigid wave-absorbing material with high temperature resistance and high thermal conductivity and a preparation method thereof, so as to meet the thermal conductivity requirement of high-power microwave devices/products on the wave-absorbing material.
Disclosure of Invention
The invention provides a high-temperature-resistant high-heat-conductivity rigid wave-absorbing material and a preparation method thereof. The high-temperature-resistant high-heat-conductivity wave-absorbing material has excellent high-temperature resistance, heat-conductivity performance and microwave absorption performance.
In a first aspect, the invention provides a preparation method of a rigid wave-absorbing material with high temperature resistance and high heat conduction, which comprises the following steps:
(1) Mixing the ferrosilicon-chromium alloy powder with boric acid, fully stirring, and then placing the mixture in a planetary ball mill for ball milling to obtain mixed powder;
(2) Placing the ball-milled mixed powder into a high-temperature sintering furnace, and sintering in an ammonia atmosphere to obtain boron nitride coated ferrosilicon chromium alloy powder;
(3) And uniformly mixing the obtained coated ferrosilicon chromium alloy powder with propargyl phenolic resin, and curing and forming the mixture in a mold to obtain the high-temperature-resistant high-heat-conductivity rigid wave-absorbing material.
Preferably, the mass ratio of the ferrosilicon chromium alloy powder to the boric acid in the step (1) is (1-1.5): 1.
Preferably, the grain size of the ferrosilicon chromium alloy powder in the step (1) is 5-10 mu m.
Preferably, the ball milling time in step (1) is 6-8 hours.
Preferably, the sintering temperature in step (2) is 800-900 ℃.
Preferably, the sintering time in step (2) is 4-6 hours.
Preferably, in the step (3), the mass ratio of the ferrosilicon chromium alloy powder to the propargyl phenolic resin is 8:2-9:1.
Preferably, the curing procedure in step (3) is 160 ℃/2 hours, 180 ℃/2 hours, 200 ℃/2 hours and 230 ℃/1 hour.
In a second aspect, the invention provides a high-temperature-resistant high-thermal-conductivity rigid wave-absorbing material prepared by the preparation method in any one of the first aspects.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) According to the invention, the boron nitride coated ferrosilicon chromium alloy powder is modified to prepare the wave-absorbing material, so that the wave-absorbing material has excellent heat conduction performance and high temperature resistance, and the use condition of the material is expanded.
(2) The high-temperature-resistant high-heat-conductivity rigid wave-absorbing material can meet the requirements of aviation and aerospace craft antennas and the like on the high-performance rigid wave-absorbing material.
(3) The invention is different from CN109326405A in that the propargyl phenolic resin is special modified resin, and the temperature resistance is far higher than that of the conventional phenolic resin, so as to prepare the rigid wave-absorbing material with high temperature resistance and high heat conductivity. The invention is different from the patent CN111234777A in that the ball milling and sintering cladding mode and the powder outer layer cladding structure are directly utilized; the propargyl phenolic resin is an organic binder, can be self-catalyzed and solidified without a curing agent, and is a high-temperature-resistant high-heat-conductivity rigid wave-absorbing material prepared by pouring. The invention is different from the patent CN115365488A in that propargyl phenolic resin is used for preparing the wave-absorbing material with better temperature resistance and high heat conduction performance. The invention is different from the patent CN116102791A in that the high-temperature-resistant high-heat-conductivity rigid wave-absorbing material is prepared by directly utilizing a ball milling and sintering cladding mode and a powder outer layer cladding structure. The invention is different from the patent CN116156858A in that boron nitride is adopted to coat the surface of the ferrosilicon chromium powder, and different coating processes are adopted; the binder is propargyl phenolic resin, has high glass transition temperature, and the prepared wave-absorbing material has different performances. The invention is different from the patent CN116179118A in ball milling coating modification mode, the used adhesive is different, and the prepared wave-absorbing material has different heat conducting properties.
Drawings
FIG. 1 is an SEM image of a ferrosilicon chromium alloy powder prior to boron nitride coating;
FIG. 2 is an SEM image of the iron-silicon-chromium alloy powder after coating with boron nitride;
fig. 3 is a graph showing the comparison of the thermal conductivity coefficients of the wave-absorbing materials obtained by coating the ferrosilicon-chromium alloy powder with boron nitride.
Detailed Description
In order to make the technical features and advantages or technical effects of the technical scheme of the invention more obvious and understandable, the following detailed description is given with reference to the accompanying drawings.
The invention provides a high-temperature-resistant high-heat-conductivity rigid wave-absorbing material and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) Mixing the ferrosilicon-chromium alloy powder with boric acid, fully stirring, and then placing the mixture in a planetary ball mill for ball milling to obtain mixed powder;
(2) Placing the ball-milled mixed powder into a high-temperature sintering furnace, and sintering in an ammonia atmosphere to obtain boron nitride coated ferrosilicon chromium alloy powder;
(3) And uniformly mixing the obtained coated alloy powder with propargyl phenolic resin, and curing and forming the mixture in a mold to obtain the high-temperature-resistant high-heat-conductivity rigid wave-absorbing material.
According to some preferred embodiments, in step (1), the mass ratio of the ferrosilicon chromium alloy powder to boric acid is (1-1.5): 1 (e.g., may be 1:1, 1.1:1, 1.2:1, 1.3:1, 1.4:1, 1.5:1)
According to some more preferred embodiments, the ferrosilicon chromium alloy powder has a particle size of 5-10 μm (e.g., may be 5 μm, 6 μm, 7 μm, 8 μm, 9 μm, or 10 μm).
According to some more preferred embodiments, the ball milling time is 6-8 hours (e.g., may be 6 hours, 7 hours, or 8 hours).
According to some preferred embodiments, in step (2), the sintering temperature is 800-900 ℃ (e.g. may be 800 ℃, 850 ℃ or 900 ℃).
According to some more preferred embodiments, the sintering time is 4-6 hours (e.g., may be 4 hours, 5 hours, or 6 hours).
According to some preferred embodiments, in step (3), the mass ratio of the clad alloy powder to the propargyl phenolic resin is from 8:2 to 9:1 (e.g. may be 8:2, 8.5:1.5 or 9:1).
According to some preferred embodiments, in step (3), the curing procedure is 160 ℃/2h,180 ℃/2h,200 ℃/2h and 230 ℃/1h.
In order to more clearly illustrate the technical scheme and advantages of the invention, the following describes a high-temperature-resistant and high-heat-conductivity rigid wave-absorbing material and a preparation method thereof in detail through a plurality of embodiments.
Example 1
(1) Mixing ferrosilicon-chromium alloy powder (particle size 10 mu m,100 g) and boric acid (100 g), fully stirring, and then placing in a planetary ball mill for ball milling for 6 hours to obtain mixed powder;
(2) Placing the ball-milled mixed powder into a high-temperature sintering furnace, and sintering in an ammonia atmosphere at 800 ℃ for 4 hours to obtain boron nitride coated ferrosilicon chromium alloy powder;
(3) And uniformly mixing 80g of coated alloy powder with 20g of propargyl phenolic resin, and then placing the mixture into a die, and curing and molding according to curing procedures of 160 ℃/2h,180 ℃/2h,200 ℃/2h and 230 ℃/1h to obtain the high-temperature-resistant high-heat-conductivity rigid wave-absorbing material.
Example 2
Example 2 is substantially the same as example 1 except that: the grain size of the ferrosilicon chromium alloy powder is 5 mu m and 120g.
Example 3
Example 3 is substantially the same as example 1 except that: the mass of the ferrosilicon chromium alloy powder is 8 mu m and 150g.
Example 4
Example 4 is substantially the same as example 1 except that: the ball milling time was 8 hours and the sintering temperature was 850 ℃.
Example 5
Example 5 is substantially the same as example 1 except that: the ball milling time was 7 hours, the sintering temperature was 900℃and the sintering time was 5 hours.
Example 6
Example 6 is substantially the same as example 1 except that: the sintering time is 6 hours, the alloy powder after coating is 85g, and the propargyl phenolic resin is 15g.
Example 7
Example 7 is substantially the same as example 1 except that: the alloy powder after coating is 90g, and the propargyl phenolic resin is 10g.
Comparative example 1
(1) Mixing ferrosilicon-chromium alloy powder (particle size of 20 mu m,100 g) and boric acid (100 g), fully stirring, and then placing in a planetary ball mill for ball milling for 6 hours to obtain mixed powder;
(2) Placing the ball-milled mixed powder into a high-temperature sintering furnace, and sintering in an ammonia atmosphere at 800 ℃ for 4 hours to obtain boron nitride coated ferrosilicon chromium alloy powder;
(3) And uniformly mixing 80g of coated alloy powder with 20g of propargyl phenolic resin, and then placing the mixture into a die, and curing and molding according to curing procedures of 160 ℃/2h,180 ℃/2h,200 ℃/2h and 230 ℃/1h to obtain the high-temperature-resistant high-heat-conductivity rigid wave-absorbing material.
Comparative example 2
(1) Mixing ferrosilicon-chromium alloy powder (particle size 10 mu m,200 g) and boric acid (100 g), fully stirring, and then placing in a planetary ball mill for ball milling for 6 hours to obtain mixed powder;
(2) Placing the ball-milled mixed powder into a high-temperature sintering furnace, and sintering in an ammonia atmosphere at 800 ℃ for 4 hours to obtain boron nitride coated ferrosilicon chromium alloy powder;
(3) And uniformly mixing 80g of coated alloy powder with 20g of propargyl phenolic resin, and then placing the mixture into a die, and curing and molding according to curing procedures of 160 ℃/2h,180 ℃/2h,200 ℃/2h and 230 ℃/1h to obtain the high-temperature-resistant high-heat-conductivity rigid wave-absorbing material.
Comparative example 3
(1) Mixing ferrosilicon-chromium alloy powder (particle size 10 mu m,100 g) and boric acid (100 g), fully stirring, and then placing in a planetary ball mill for ball milling for 1 hour to obtain mixed powder;
(2) Placing the ball-milled mixed powder into a high-temperature sintering furnace, and sintering in an ammonia atmosphere at 800 ℃ for 4 hours to obtain boron nitride coated ferrosilicon chromium alloy powder;
(3) And uniformly mixing 80g of coated alloy powder with 20g of propargyl phenolic resin, and then placing the mixture into a die, and curing and molding according to curing procedures of 160 ℃/2h,180 ℃/2h,200 ℃/2h and 230 ℃/1h to obtain the high-temperature-resistant high-heat-conductivity rigid wave-absorbing material.
Comparative example 4
(1) Mixing ferrosilicon-chromium alloy powder (particle size 10 mu m,100 g) and boric acid (100 g), fully stirring, and then placing in a planetary ball mill for ball milling for 6 hours to obtain mixed powder;
(2) Placing the ball-milled mixed powder into a high-temperature sintering furnace, and sintering in an ammonia atmosphere at 600 ℃ for 4 hours to obtain boron nitride coated ferrosilicon chromium alloy powder;
(3) And uniformly mixing 80g of coated alloy powder with 20g of propargyl phenolic resin, and then placing the mixture into a die, and curing and molding according to curing procedures of 160 ℃/2h,180 ℃/2h,200 ℃/2h and 230 ℃/1h to obtain the high-temperature-resistant high-heat-conductivity rigid wave-absorbing material.
Comparative example 5
(1) Mixing ferrosilicon-chromium alloy powder (particle size 10 mu m,100 g) and boric acid (100 g), fully stirring, and then placing in a planetary ball mill for ball milling for 6 hours to obtain mixed powder;
(2) Placing the ball-milled mixed powder into a high-temperature sintering furnace, and sintering in an ammonia atmosphere at 800 ℃ for 1 hour to obtain boron nitride coated ferrosilicon chromium alloy powder;
(3) And uniformly mixing 80g of coated alloy powder with 20g of propargyl phenolic resin, and then placing the mixture into a die, and curing and molding according to curing procedures of 160 ℃/2h,180 ℃/2h,200 ℃/2h and 230 ℃/1h to obtain the high-temperature-resistant high-heat-conductivity rigid wave-absorbing material.
Comparative example 6
(1) Mixing ferrosilicon-chromium alloy powder (particle size 10 mu m,100 g) and boric acid (100 g), fully stirring, and then placing in a planetary ball mill for ball milling for 6 hours to obtain mixed powder;
(2) Placing the ball-milled mixed powder into a high-temperature sintering furnace, and sintering in an ammonia atmosphere at 800 ℃ for 4 hours to obtain boron nitride coated ferrosilicon chromium alloy powder;
(3) And uniformly mixing 70g of the coated alloy powder with 30g of propargyl phenolic resin, and then placing the mixture into a die, and curing and molding according to curing procedures of 160 ℃/2h,180 ℃/2h,200 ℃/2h and 230 ℃/1h to obtain the high-temperature-resistant high-heat-conductivity rigid wave-absorbing material.
Fig. 1 is an SEM image of the ferrosilicon chromium alloy powder before the coating of the boron nitride in example 1, and fig. 2 is an SEM image of the ferrosilicon chromium alloy powder after the coating of the boron nitride in example 1, and it can be seen that a layer of boron nitride is coated on the surface of the ferrosilicon chromium alloy powder after the treatment of example 1.
The high-temperature-resistant, high-thermal-conductivity rigid wave-absorbing materials obtained in examples 1 to 7 and comparative examples 1 to 6 were respectively tested for thermal conductivity and glass transition temperature. Specifically, the thermal conductivity was tested: test pieces 50.8mm in diameter were machined according to standard machines and tested for thermal conductivity, glass transition temperature: the glass transition temperature was measured by DMA according to standard machine addition of 80X 10X 4mm samples.
Fig. 3 shows the thermal conductivity of the uncoated ferrosilicon chromium powder wave-absorbing material and the coated ferrosilicon chromium powder wave-absorbing material of example 5, and the thermal conductivity is greatly improved after coating.
The test results of the wave-absorbing materials prepared in all examples and comparative examples are shown in table 1 below.
Table 1 coefficient of thermal conductivity of the wave-absorbing material prepared after modification of the thermally conductive filler
| Project | Coefficient of thermal conductivity (W/(m. K)) | Glass transition temperature (. Degree. C.) |
| Example 1 | 2.4 | 285℃ |
| Example 2 | 2.3 | 283℃ |
| Example 3 | 2.1 | 290℃ |
| Example 4 | 2.4 | 278℃ |
| Example 5 | 2.5 | 284℃ |
| Example 6 | 2.2 | 275℃ |
| Example 7 | 2.6 | 291℃ |
| Comparative example 1 | 1.6 | 288℃ |
| Comparative example 2 | 1.5 | 292℃ |
| Comparative example 3 | 1.3 | 281℃ |
| Comparative example 4 | 1.1 | 286℃ |
| Comparative example 5 | 1.2 | 279℃ |
| Comparative example 6 | 1.4 | 277℃ |
As can be seen from table 1, the heat conductivity coefficient of the wave-absorbing material prepared in the embodiment of the invention is significantly better than that of the comparative example, which indicates that the technical scheme of the invention can prepare the wave-absorbing material with excellent heat conductivity.
Although the present invention has been described with reference to the above embodiments, it should be understood that the invention is not limited thereto, and that modifications and equivalents may be made thereto by those skilled in the art, which modifications and equivalents are intended to be included within the scope of the present invention as defined by the appended claims.
Claims (9)
1. The preparation method of the rigid wave-absorbing material with high temperature resistance and high heat conduction is characterized by comprising the following steps:
(1) Mixing the ferrosilicon-chromium alloy powder with boric acid, fully stirring, and then placing the mixture in a planetary ball mill for ball milling to obtain mixed powder;
(2) Placing the ball-milled mixed powder into a high-temperature sintering furnace, and sintering in an ammonia atmosphere to obtain boron nitride coated ferrosilicon chromium alloy powder;
(3) And uniformly mixing the obtained coated ferrosilicon chromium alloy powder with propargyl phenolic resin, and curing and forming the mixture in a mold to obtain the high-temperature-resistant high-heat-conductivity rigid wave-absorbing material.
2. The method according to claim 1, wherein the mass ratio of the Fe-Si-Cr alloy powder to the boric acid in the step (1) is 1-1.5:1.
3. The method according to claim 1, wherein the ferrosilicon-chromium alloy powder in the step (1) has a particle size of 5 to 10. Mu.m.
4. The method according to claim 1, wherein the ball milling time in the step (1) is 6 to 8 hours.
5. The method of claim 1, wherein the sintering temperature in step (2) is 800-900 ℃.
6. The method of claim 1, wherein the sintering time in step (2) is 4 to 6 hours.
7. The preparation method of claim 1, wherein the mass ratio of the ferrosilicon chromium alloy powder to the propargyl phenolic resin in the step (3) is 8:2-9:1.
8. The method of claim 1, wherein the curing procedure in step (3) is 160 ℃/2 hours, 180 ℃/2 hours, 200 ℃/2 hours and 230 ℃/1 hour.
9. A rigid wave-absorbing material with high temperature resistance and high heat conductivity, which is characterized in that the material is prepared by the preparation method of any one of claims 1-8.
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