CN113214655A - Electromagnetic shielding wave-absorbing heat-conducting film - Google Patents
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Abstract
The invention relates to the technical field of electromagnetic shielding films and discloses an electromagnetic shielding wave-absorbing heat-conducting film, wherein epoxy resin is added into a composite film to graft nano Fe3O4The Co-doped flower-spherical tin dioxide can obviously increase the electromagnetic wave absorption rate and the thermal conductivity of the film, the ferroferric oxide and the tin dioxide have a synergistic effect, the electromagnetic wave absorption capacity of the film is increased, when the ferroferric oxide is grafted on epoxy resin, the ferroferric oxide is uniformly distributed in the epoxy resin, the magnetic resonance peak of the wave absorber gradually moves to a high-frequency region, and the flower-spherical shape increases the ratio of the tin dioxideThe surface area is increased, the wave absorbing efficiency of the wave absorbing material is improved, Co-doped tin dioxide is used, the wave absorbing capacity of the film is further improved, ferroferric oxide also has a heat conducting effect, and the heat conductivity of the film is improved through an organic-inorganic chain or network structure.
Description
Technical Field
The invention relates to the technical field of electromagnetic shielding films, in particular to an electromagnetic shielding wave-absorbing heat-conducting film.
Background
With the rapid development of electronic technology, communication networks and electronic devices such as televisions, computers and mobile phones have become more and more closely related to us, when these devices transmit or receive electrical signals, they inevitably generate electromagnetic waves, which, on the one hand, as electronic devices operate at higher and higher frequencies, and their component sizes are continually shrinking, excessive electromagnetic radiation contamination can adversely affect the reliability and useful life of electronic products, and, on the other hand, as electromagnetic radiation continues to penetrate our lives, the potential health influence of the electromagnetic shielding wave-absorbing material draws great attention of people, so that the development of the effective electromagnetic shielding wave-absorbing material has important significance for reducing or eliminating electromagnetic radiation pollution, in addition, the high integration of electronic products leads to the increase of heat productivity, and the wave-absorbing material needs to have certain heat conductivity.
As is well known, electromagnetic wave shielding is mainly composed of absorption and reflection aspects, and typical electromagnetic wave shielding materials have key requirements of low density, high electrical conductivity and excellent thermal stability, among various electromagnetic wave shielding materials, composite materials based on conductive polymers are main candidate materials to replace metal similar materials thereof, mainly due to their advantages of light weight, excellent formability, excellent chemical stability and convenient design flexibility, although a large portion of electromagnetic wave shielding materials are reflected, which may cause secondary electromagnetic wave pollution, and it is really necessary to develop a highly efficient electromagnetic wave shielding material with good absorbability, and ferroferric oxide is one of the most widely used metal oxide materials, has the advantages of low price, low toxicity, good biocompatibility and the like, and is widely used in sensors, biomedicine, magnetic recording devices, environmental management, food testing and other fields, and more importantly, it can provide magnetic loss and have a certain thermal conductivity in electromagnetic wave composites, but agglomeration is also a problem that ferroferric oxide is required to face, since ferroferric oxide nanoparticles can easily agglomerate to form large magnets, thereby losing their superparamagnetism, ferroferric oxide nanoparticles exposed to air are easily oxidized and lose magnetism, tin dioxide is attracting attention due to its excellent properties, such as good chemical and thermal stability, low cost, wide band gap and dielectric loss characteristics, and doping metal ions is a useful method to enhance the absorption properties of semiconductor compound related composites by adjusting electromagnetic parameters to improve impedance matching.
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides an electromagnetic shielding wave-absorbing heat-conducting film, which solves the problems of poor wave-absorbing performance and low heat conductivity of a pure epoxy resin film.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: the preparation method of the electromagnetic shielding wave-absorbing heat-conducting film comprises the following steps:
(1) modifying the nano ferroferric oxide by mercaptopropyl methyldimethoxysilane to obtain the sulfhydrylated nano ferroferric oxide;
(2) dissolving sulfhydrylated nano ferroferric oxide and triethylamine in cyclohexane, then adding dichlorodimethylsilane, stirring uniformly, carrying out substitution reaction, after the reaction is finished, filtering, washing by using cyclohexane and deionized water, and drying to obtain chloro-dimethylsilyl nano ferroferric oxide;
(3) adding epoxy resin and chloro-dimethylsilyl nano ferroferric oxide into a reaction bottle for substitution reaction, adding triethylamine for neutralization after the reaction is finished, filtering, washing and drying to obtain epoxy resin grafted nano ferroferric oxide;
(4) dissolving tin tetrachloride and cobalt chloride in deionized water, then adding sodium hydroxide and polyvinylpyrrolidone, stirring uniformly, transferring to a reaction kettle, carrying out hydrothermal reaction, after the reaction is finished, filtering, washing with ethanol and deionized water, and drying to obtain Co-doped flower-ball-shaped tin dioxide;
(5) uniformly dispersing epoxy resin grafted nano ferroferric oxide and Co-doped flower-ball-shaped tin dioxide in an ethylene-propylene ketone solvent, adding a curing agent methyl hexahydrophthalic anhydride and a promoter 2-ethyl 4-methylimidazole, uniformly stirring, preparing a smear from the mixed solution by using a spin coater, and drying after the solvent is completely volatilized to obtain the electromagnetic shielding wave-absorbing heat-conducting film.
Preferably, the mass ratio of the sulfhydrylated nano ferroferric oxide, the triethylamine and the dichlorodimethylsilane in the step (2) is 100:30-45: 20-30.
Preferably, the reaction temperature of the substitution reaction in the step (2) is 50-80 ℃, and the reaction time is 12-36 h.
Preferably, in the step (3), the mass ratio of the epoxy resin to the chlorodimethylsilyl nano ferroferric oxide is 100:4-10: 3-7.
Preferably, the reaction temperature of the substitution reaction in the step (3) is 20-40 ℃, and the reaction time is 1-3 h.
Preferably, the mass ratio of the tin tetrachloride, the cobalt chloride, the sodium hydroxide and the polyvinylpyrrolidone in the step (4) is 100:1.5-2.5: 110-.
Preferably, the reaction temperature of the hydrothermal reaction in the step (4) is 180-220 ℃, and the reaction time is 18-30 h.
Preferably, in the step (5), the epoxy resin grafted nano ferroferric oxide, the Co-doped flower-ball-shaped tin dioxide, the methyl hexahydrophthalic anhydride and the 2-ethyl-4-methylimidazole have a mass ratio of 100:2-5:60-90: 1-3.
(III) advantageous technical effects
Compared with the prior art, the invention has the following experimental principles and beneficial technical effects:
the electromagnetic shielding wave-absorbing heat-conducting film is characterized in that mercaptopropyl methyldimethoxysilane is used for modifying nano ferroferric oxide to obtain mercaptolated nano ferroferric oxide, then, under the catalytic action of triethylamine, the mercapto group of the mercaptolated nano ferroferric oxide and the chlorine atom of dichlorodimethylsilane are subjected to substitution reaction to obtain chloro-dimethylsilyl nano ferroferric oxide, then, the chlorine atom of the chloro-dimethylsilyl nano ferroferric oxide is subjected to reaction with the hydroxyl group of epoxy resin to obtain epoxy resin grafted nano ferroferric oxide, then, stannic chloride is used as a tin source, cobalt chloride is used as a cobalt source, polyvinylpyrrolidone is used as a surfactant to inhibit agglomeration among particles, hydrothermal reaction is carried out under the alkaline condition to obtain Co-doped flower-spherical tin dioxide, and finally, the epoxy resin grafted nano ferroferric oxide and the Co-doped flower-spherical tin dioxide are used as wave-absorbing and heat-conducting materials, the electromagnetic shielding wave-absorbing heat-conducting film is prepared by taking methyl hexahydrophthalic anhydride as a curing agent and 2-ethyl 4-methylimidazole as an accelerant.
Compared with the unmodified electromagnetic shielding wave absorbing heat conducting film, the electromagnetic shielding wave absorbing film prepared in the new mode has higher electromagnetic wave absorbing efficiency and heat conducting efficiency, and epoxy resin grafted nano Fe is added into the composite film3O4The Co-doped flower-spherical tin dioxide can obviously increase the electromagnetic wave absorption rate and the thermal conductivity of the film, when the ferroferric oxide and the tin dioxide are contacted in the film, the synergistic effect is generated between the ferroferric oxide and the tin dioxide, the electric conduction loss capability of the wave absorbing material is increased, when the electric conduction loss capability and the magnetic loss capability reach a relative balance state, the impedance matching performance is improved, the electromagnetic wave absorption capability of the film is increased, when the ferroferric oxide is grafted on the epoxy resin, the ferroferric oxide is uniformly distributed in the epoxy resin, the magnetic conductivity in the epoxy resin is increased, and the ferroferric oxide has high anisotropy, so when the ferroferric oxide is compounded with the tin dioxide, the magnetic resonance peak of the wave absorbing agent can gradually move to a high-frequency region, the specific surface area of the tin dioxide is increased due to the flower-spherical shape, more sites are provided for the scattering of electromagnetic waves, and more scattering behaviors can be generated for the electromagnetic waves, the consumption of incident electromagnetic waves in the film is increased, the wave absorbing efficiency of the wave absorbing material is increased, Co-doped stannic oxide is used, the magnetic loss tangent angle of the film is increased, the magnetic loss efficiency of the stannic oxide is improved, when Co atoms are doped into stannic oxide lattices, the moving speed of electrons in the Co-doped stannic oxide is increased, the Co-doped stannic oxide can improve the conductivity of the stannic oxide, the resistance is reduced, the magnetic loss mainly occurs in a high-frequency position, the wave absorbing capacity of the film is further improved, ferroferric oxide is used as the wave absorbing material and also has the function of heat conduction, and the ferroferric oxide grafted by resin in the film is in contact with other substancesAn organic-inorganic chain or network structure is formed between the substances, so that the film has a heat conduction effect, and the heat conductivity of the film is improved.
Drawings
FIG. 1 is a reaction mechanism diagram of ferroferric oxide and dichlorodimethylsilane;
FIG. 2 is a reaction mechanism diagram of chlorodimethylsilyl nano ferroferric oxide and epoxy resin.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: an electromagnetic shielding wave-absorbing heat-conducting film comprises the following steps:
(1) modifying the nano ferroferric oxide by mercaptopropyl methyldimethoxysilane to obtain the sulfhydrylated nano ferroferric oxide;
(2) according to the mass ratio of 100:30-45:20-30, dissolving sulfhydrylated nano ferroferric oxide and triethylamine in cyclohexane, adding dichlorodimethylsilane, stirring uniformly, carrying out substitution reaction at 50-80 ℃, wherein the reaction time is 12-36h, after the reaction is finished, filtering, washing with cyclohexane and deionized water, and drying to obtain chloro-dimethylsilyl nano ferroferric oxide;
(3) adding epoxy resin and chloro-dimethylsilyl nano ferroferric oxide into a reaction bottle according to the mass ratio of 100:4-10:3-7, carrying out substitution reaction at 20-40 ℃, reacting for 1-3h, adding triethylamine for neutralization after the reaction is finished, filtering, washing and drying to obtain epoxy resin grafted nano ferroferric oxide;
(4) dissolving tin tetrachloride and cobalt chloride in deionized water according to the mass ratio of 100:1.5-2.5: 110-;
(5) uniformly dispersing epoxy resin grafted nano ferroferric oxide and Co-doped flower-ball-shaped tin dioxide in an ethylene-propylene ketone solvent, adding a curing agent methyl hexahydrophthalic anhydride and an accelerant 2-ethyl 4-methylimidazole, wherein the mass ratio of the epoxy resin grafted nano ferroferric oxide to the Co-doped flower-ball-shaped tin dioxide to the methyl hexahydrophthalic anhydride to the 2-ethyl 4-methylimidazole is 100:2-5:60-90:1-3, uniformly stirring, preparing a smear from the mixed solution by using a spin coater, and drying after the solvent is volatilized to obtain the electromagnetic shielding wave-absorbing heat-conducting film.
Example 1
(1) Modifying the nano ferroferric oxide by mercaptopropyl methyldimethoxysilane to obtain the sulfhydrylated nano ferroferric oxide;
(2) according to the mass ratio of 100:30:20, dissolving sulfhydrylated nano ferroferric oxide and triethylamine in cyclohexane, adding dichlorodimethylsilane, stirring uniformly, carrying out substitution reaction at 50 ℃ for 12 hours, filtering after the reaction is finished, washing with cyclohexane and deionized water, and drying to obtain chloro-dimethylsilyl nano ferroferric oxide;
(3) adding epoxy resin and chloro-dimethylsilyl nano ferroferric oxide into a reaction bottle according to the mass ratio of 100:4:3, carrying out substitution reaction at 20 ℃, reacting for 1h, adding triethylamine for neutralization after the reaction is finished, filtering, washing and drying to obtain epoxy resin grafted nano ferroferric oxide;
(4) dissolving stannic chloride and cobalt chloride in deionized water according to the mass ratio of 100:1.5:110:120, then adding sodium hydroxide and polyvinylpyrrolidone, stirring uniformly, transferring to a reaction kettle, carrying out hydrothermal reaction at 180 ℃, wherein the reaction time is 18h, after the reaction is finished, filtering, washing with ethanol and deionized water, and drying to obtain Co-doped flower-ball-shaped stannic oxide;
(5) uniformly dispersing epoxy resin grafted nano ferroferric oxide and Co-doped flower-ball-shaped tin dioxide in an ethylene-propylene ketone solvent, adding a curing agent methyl hexahydrophthalic anhydride and an accelerant 2-ethyl 4-methylimidazole, wherein the mass ratio of the epoxy resin grafted nano ferroferric oxide to the Co-doped flower-ball-shaped tin dioxide to the methyl hexahydrophthalic anhydride to the 2-ethyl 4-methylimidazole is 100:2:60:1, uniformly stirring, preparing a smear from the mixed solution by using a spin coater, and drying after the solvent is volatilized to obtain the electromagnetic shielding wave-absorbing heat-conducting film.
Example 2
(1) Modifying the nano ferroferric oxide by mercaptopropyl methyldimethoxysilane to obtain the sulfhydrylated nano ferroferric oxide;
(2) according to the mass ratio of 100:35:22, dissolving sulfhydrylated nano ferroferric oxide and triethylamine in cyclohexane, adding dichlorodimethylsilane, stirring uniformly, carrying out substitution reaction at 60 ℃, wherein the reaction time is 18h, after the reaction is finished, filtering, washing with cyclohexane and deionized water, and drying to obtain chloro-dimethylsilyl nano ferroferric oxide;
(3) adding epoxy resin and chlorodimethylsilyl nano ferroferric oxide into a reaction bottle according to the mass ratio of 100:6:4, carrying out substitution reaction at 25 ℃, wherein the reaction time is 1.5h, adding triethylamine for neutralization after the reaction is finished, filtering, washing and drying to obtain epoxy resin grafted nano ferroferric oxide;
(4) dissolving tin tetrachloride and cobalt chloride in deionized water according to the mass ratio of 100:1.8:115:140, then adding sodium hydroxide and polyvinylpyrrolidone, uniformly stirring, transferring to a reaction kettle, carrying out hydrothermal reaction at 190 ℃, wherein the reaction time is 22h, after the reaction is finished, filtering, washing with ethanol and deionized water, and drying to obtain Co-doped flower-ball-shaped tin dioxide;
(5) uniformly dispersing epoxy resin grafted nano ferroferric oxide and Co-doped flower-ball-shaped tin dioxide in an ethylene-propylene ketone solvent, adding a curing agent methyl hexahydrophthalic anhydride and an accelerant 2-ethyl 4-methylimidazole, wherein the mass ratio of the epoxy resin grafted nano ferroferric oxide to the Co-doped flower-ball-shaped tin dioxide to the methyl hexahydrophthalic anhydride to the 2-ethyl 4-methylimidazole is 100:3:70:1.5, uniformly stirring, preparing a smear from the mixed solution by using a spin coater, and drying after the solvent is volatilized to obtain the electromagnetic shielding wave-absorbing heat-conducting film.
Example 3
(1) Modifying the nano ferroferric oxide by mercaptopropyl methyldimethoxysilane to obtain the sulfhydrylated nano ferroferric oxide;
(2) according to the mass ratio of 100:40:26, dissolving sulfhydrylated nano ferroferric oxide and triethylamine in cyclohexane, adding dichlorodimethylsilane, stirring uniformly, carrying out substitution reaction at 70 ℃, wherein the reaction time is 30h, after the reaction is finished, filtering, washing with cyclohexane and deionized water, and drying to obtain chloro-dimethylsilyl nano ferroferric oxide;
(3) adding epoxy resin and chloro-dimethylsilyl nano ferroferric oxide into a reaction bottle according to the mass ratio of 100:8:6, carrying out substitution reaction at 35 ℃ for 2h, adding triethylamine for neutralization after the reaction is finished, filtering, washing and drying to obtain epoxy resin grafted nano ferroferric oxide;
(4) dissolving tin tetrachloride and cobalt chloride in deionized water according to the mass ratio of 100:2.2:120:160, then adding sodium hydroxide and polyvinylpyrrolidone, uniformly stirring, transferring to a reaction kettle, carrying out hydrothermal reaction at 210 ℃, reacting for 26 hours, after the reaction is finished, filtering, washing with ethanol and deionized water, and drying to obtain Co-doped flower-ball-shaped tin dioxide;
(5) uniformly dispersing epoxy resin grafted nano ferroferric oxide and Co-doped flower-ball-shaped tin dioxide in an ethylene-propylene ketone solvent, adding a curing agent methyl hexahydrophthalic anhydride and an accelerant 2-ethyl 4-methylimidazole, wherein the mass ratio of the epoxy resin grafted nano ferroferric oxide to the Co-doped flower-ball-shaped tin dioxide to the methyl hexahydrophthalic anhydride to the 2-ethyl 4-methylimidazole is 100:4:80:2.5, uniformly stirring, preparing a smear from the mixed solution by using a spin coater, and drying after the solvent is volatilized to obtain the electromagnetic shielding wave-absorbing heat-conducting film.
Example 4
(1) Modifying the nano ferroferric oxide by mercaptopropyl methyldimethoxysilane to obtain the sulfhydrylated nano ferroferric oxide;
(2) according to the mass ratio of 100:45:30, dissolving sulfhydrylated nano ferroferric oxide and triethylamine in cyclohexane, adding dichlorodimethylsilane, stirring uniformly, carrying out substitution reaction at 80 ℃ for 36h, filtering after the reaction is finished, washing with cyclohexane and deionized water, and drying to obtain chloro-dimethylsilyl nano ferroferric oxide;
(3) adding epoxy resin and chloro-dimethylsilyl nano ferroferric oxide into a reaction bottle according to the mass ratio of 100:10:7, carrying out substitution reaction at 40 ℃, reacting for 3 hours, adding triethylamine for neutralization after the reaction is finished, filtering, washing and drying to obtain epoxy resin grafted nano ferroferric oxide;
(4) dissolving stannic chloride and cobalt chloride in deionized water according to the mass ratio of 100:2.5:130:180, then adding sodium hydroxide and polyvinylpyrrolidone, stirring uniformly, transferring to a reaction kettle, carrying out hydrothermal reaction at 220 ℃, wherein the reaction time is 30 hours, after the reaction is finished, filtering, washing with ethanol and deionized water, and drying to obtain Co-doped flower-ball-shaped stannic oxide;
(5) uniformly dispersing epoxy resin grafted nano ferroferric oxide and Co-doped flower-ball-shaped tin dioxide in an ethylene-propylene ketone solvent, adding a curing agent methyl hexahydrophthalic anhydride and an accelerant 2-ethyl 4-methylimidazole, wherein the mass ratio of the epoxy resin grafted nano ferroferric oxide to the Co-doped flower-ball-shaped tin dioxide to the methyl hexahydrophthalic anhydride to the 2-ethyl 4-methylimidazole is 100:5:90:3, uniformly stirring, preparing a smear from the mixed solution by using a spin coater, and drying after the solvent is volatilized to obtain the electromagnetic shielding wave-absorbing heat-conducting film.
Comparative example 1
(1) Modifying the nano ferroferric oxide by mercaptopropyl methyldimethoxysilane to obtain the sulfhydrylated nano ferroferric oxide;
(2) according to the mass ratio of 100:20:14, dissolving sulfhydrylated nano ferroferric oxide and triethylamine in cyclohexane, adding dichlorodimethylsilane, stirring uniformly, carrying out substitution reaction at 35 ℃ for 8 hours, filtering after the reaction is finished, washing with cyclohexane and deionized water, and drying to obtain chloro-dimethylsilyl nano ferroferric oxide;
(3) adding epoxy resin and chlorodimethylsilyl nano ferroferric oxide into a reaction bottle according to the mass ratio of 100:3:2, carrying out substitution reaction at 14 ℃, wherein the reaction time is 0.7h, adding triethylamine for neutralization after the reaction is finished, filtering, washing and drying to obtain epoxy resin grafted nano ferroferric oxide;
(4) dissolving tin tetrachloride and cobalt chloride in deionized water according to the mass ratio of 100:1.0:75:80, then adding sodium hydroxide and polyvinylpyrrolidone, stirring uniformly, transferring to a reaction kettle, carrying out hydrothermal reaction at 120 ℃, reacting for 12h, after the reaction is finished, filtering, washing with ethanol and deionized water, and drying to obtain Co-doped flower-ball-shaped tin dioxide;
(5) uniformly dispersing epoxy resin grafted nano ferroferric oxide and Co-doped flower-ball-shaped tin dioxide in an ethylene-propylene ketone solvent, adding a curing agent methyl hexahydrophthalic anhydride and an accelerant 2-ethyl 4-methylimidazole, wherein the mass ratio of the epoxy resin grafted nano ferroferric oxide to the Co-doped flower-ball-shaped tin dioxide to the methyl hexahydrophthalic anhydride to the 2-ethyl 4-methylimidazole is 100:1.4:40:0.7, uniformly stirring, preparing a smear from the mixed solution by using a spin coater, and drying after the solvent is volatilized to obtain the electromagnetic shielding wave-absorbing heat-conducting film.
Comparative example 2
(1) Modifying the nano ferroferric oxide by mercaptopropyl methyldimethoxysilane to obtain the sulfhydrylated nano ferroferric oxide;
(2) according to the mass ratio of 100:60:40, dissolving sulfhydrylated nano ferroferric oxide and triethylamine in cyclohexane, adding dichlorodimethylsilane, stirring uniformly, carrying out substitution reaction at 110 ℃, filtering after the reaction is finished, washing with cyclohexane and deionized water, and drying to obtain chloro-dimethylsilyl nano ferroferric oxide;
(3) adding epoxy resin and chlorodimethylsilyl nano ferroferric oxide into a reaction bottle according to the mass ratio of 100:13:9, carrying out substitution reaction at 55 ℃, reacting for 4 hours, adding triethylamine for neutralization after the reaction is finished, filtering, washing and drying to obtain epoxy resin grafted nano ferroferric oxide;
(4) dissolving tin tetrachloride and cobalt chloride in deionized water according to a mass ratio of 100:3.2:165:240, then adding sodium hydroxide and polyvinylpyrrolidone, uniformly stirring, transferring to a reaction kettle, carrying out hydrothermal reaction at 290 ℃, wherein the reaction time is 40h, after the reaction is finished, filtering, washing with ethanol and deionized water, and drying to obtain Co-doped flower-ball-shaped tin dioxide;
(5) uniformly dispersing epoxy resin grafted nano ferroferric oxide and Co-doped flower-ball-shaped tin dioxide in an ethylene-propylene ketone solvent, adding a curing agent methyl hexahydrophthalic anhydride and an accelerant 2-ethyl 4-methylimidazole, wherein the mass ratio of the epoxy resin grafted nano ferroferric oxide to the Co-doped flower-ball-shaped tin dioxide to the methyl hexahydrophthalic anhydride to the 2-ethyl 4-methylimidazole is 100:7:120:4, uniformly stirring, preparing a smear from the mixed solution by using a spin coater, and drying after the solvent is volatilized to obtain the electromagnetic shielding wave-absorbing heat-conducting film.
The method comprises the steps of carrying out wave absorption rate test on the film material by using an arch method, firstly fixing a sample, adjusting the incident angle of an emitting source, transmitting a microwave signal, then receiving the signal by using a receiving antenna, and comparing the intensity difference of the received and transmitted microwaves to obtain the absorption rate of the film material.
The LFA 1000 laser thermal conductivity instrument is used for testing the thermal conductivity of the film material, and the cooling gas is liquid nitrogen.
Claims (8)
1. An electromagnetic shielding wave-absorbing heat-conducting film is characterized in that: the preparation method of the electromagnetic shielding wave-absorbing heat-conducting film comprises the following steps:
(1) modifying the nano ferroferric oxide by mercaptopropyl methyldimethoxysilane to obtain the sulfhydrylated nano ferroferric oxide;
(2) dissolving sulfhydrylated nano ferroferric oxide and triethylamine in cyclohexane, then adding dichlorodimethylsilane, stirring uniformly, carrying out substitution reaction, and obtaining chloro-dimethylsilyl nano ferroferric oxide after the reaction is finished;
(3) adding epoxy resin and chloro-dimethylsilyl nano ferroferric oxide into a reaction bottle for substitution reaction, and adding triethylamine for neutralization after the reaction is finished to obtain epoxy resin grafted nano ferroferric oxide;
(4) dissolving tin tetrachloride and cobalt chloride in deionized water, then adding sodium hydroxide and polyvinylpyrrolidone, uniformly stirring, transferring to a reaction kettle, carrying out hydrothermal reaction, and obtaining Co-doped flower-ball-shaped tin dioxide after the reaction is finished;
(5) uniformly dispersing epoxy resin grafted nano ferroferric oxide and Co-doped flower-ball-shaped tin dioxide in an ethylene-propylene ketone solvent, adding a curing agent methyl hexahydrophthalic anhydride and a promoter 2-ethyl 4-methylimidazole, uniformly stirring, preparing a smear from the mixed solution by using a spin coater, and drying after the solvent is completely volatilized to obtain the electromagnetic shielding wave-absorbing heat-conducting film.
2. The electromagnetic shielding wave-absorbing heat-conducting film according to claim 1, wherein: in the step (2), the mass ratio of the sulfhydrylated nano ferroferric oxide to the triethylamine to the dichlorodimethylsilane is 100:30-45: 20-30.
3. The electromagnetic shielding wave-absorbing heat-conducting film according to claim 1, wherein: the reaction temperature of the substitution reaction in the step (2) is 50-80 ℃, and the reaction time is 12-36 h.
4. The electromagnetic shielding wave-absorbing heat-conducting film according to claim 1, wherein: in the step (3), the mass ratio of the epoxy resin to the chlorodimethylsilyl nano ferroferric oxide is 100:4-10: 3-7.
5. The electromagnetic shielding wave-absorbing heat-conducting film according to claim 1, wherein: the reaction temperature of the substitution reaction in the step (3) is 20-40 ℃, and the reaction time is 1-3 h.
6. The electromagnetic shielding wave-absorbing heat-conducting film according to claim 1, wherein: the mass ratio of the tin tetrachloride, the cobalt chloride, the sodium hydroxide and the polyvinylpyrrolidone in the step (4) is 100:1.5-2.5: 110-.
7. The electromagnetic shielding wave-absorbing heat-conducting film according to claim 1, wherein: the reaction temperature of the hydrothermal reaction in the step (4) is 180-220 ℃, and the reaction time is 18-30 h.
8. The electromagnetic shielding wave-absorbing heat-conducting film according to claim 1, wherein: in the step (5), the epoxy resin grafted nano ferroferric oxide, the Co-doped flower-ball-shaped tin dioxide, the methyl hexahydrophthalic anhydride and the 2-ethyl 4-methylimidazole have a mass ratio of 100:2-5:60-90: 1-3.
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| CN202110569364.1A CN113214655A (en) | 2021-05-25 | 2021-05-25 | Electromagnetic shielding wave-absorbing heat-conducting film |
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| CN113882144A (en) * | 2021-11-02 | 2022-01-04 | 广东鹏运实业有限公司 | Anti-electromagnetic radiation fabric with surface coated with nano wave absorber and preparation method thereof |
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| CN113882144A (en) * | 2021-11-02 | 2022-01-04 | 广东鹏运实业有限公司 | Anti-electromagnetic radiation fabric with surface coated with nano wave absorber and preparation method thereof |
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