CN114190066A - High-surface-resistivity wave-absorbing material and preparation method thereof - Google Patents
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Abstract
The invention discloses a high surface resistivity wave-absorbing material and a preparation method thereof, which are characterized by comprising the following raw materials in parts by weight: 80-90 parts of absorbent, 50-70 parts of solvent type thermoplastic elastomer solution for bonding, 70-100 parts of solvent, 0.2-0.8 part of surfactant, 0.1-0.4 part of defoaming agent and 0.3-1.2 parts of cross-linking agent, wherein the preparation method comprises the steps of weighing the absorbent, the solvent, the surfactant, the solvent type thermoplastic elastomer for bonding, the defoaming agent and the cross-linking agent, and uniformly stirring and dispersing; coating the slurry on a PET release film on a coating machine, drying and volatilizing the solvent to obtain a sheet coating or a roll coating with the thickness of 50-250 um; finally, hot pressing is carried out to ensure that the cross-linking is compact, and the high-surface-resistivity wave-absorbing material is obtained.
Description
Technical Field
The invention relates to the field of electromagnetic interference and electromagnetic compatibility, in particular to a high-surface-resistivity wave-absorbing material and a preparation method thereof.
Background
With the rapid development of information technology, electronic products are developed to high frequency, micro size and integration, and electromagnetic interference and electromagnetic radiation pollution are more serious. The wave-absorbing material can absorb electromagnetic waves incident to the surface of the wave-absorbing material and then convert the electromagnetic waves into heat energy or energy in other forms, and can effectively solve the problems of electromagnetic interference and electromagnetic radiation pollution. The wave-absorbing material mainly comprises an absorbent and a binder, wherein the absorbent is flaky soft magnetic powder, the binder is generally a thermoplastic elastomer, the flakiness of the absorbent can improve the magnetic conductivity, and further the absorption efficiency is improved, the higher the flakiness degree of the absorbent is, the higher the dielectric constant is, the lower the surface resistivity is, which is not favorable for impedance matching, and in addition, the wave-absorbing material is used as a patch type material and directly attached to the surface of a chip, and if the surface resistivity is too low, the short circuit of the chip is easily caused.
The main process for improving the surface resistivity of the wave-absorbing material at present comprises the following steps: the absorbent is coated by the coupling agent, the surface resistivity of the coupling agent coated is improved to a certain extent, but the magnetic conductivity of the wave absorbing material is greatly reduced, in addition, the coating process needs to firstly dilute the coupling agent by water and alcohol, then add the absorbent into the coupling agent diluent for reaction, special equipment is needed, and the diluent needs to be dried after coating, so that the time is consumed, and the environment is polluted.
Disclosure of Invention
The invention aims to provide a high-surface-resistivity wave-absorbing material which has the advantages of time saving, cost reduction, environmental protection, greatly improved surface resistivity and basically unaffected magnetic conductivity and a preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems is as follows: a high surface resistivity wave-absorbing material is composed of the following raw materials in parts by weight: 80-90 parts of absorbent, 50-70 parts of bonding solvent type thermoplastic elastomer solution, 70-100 parts of solvent, 0.2-0.8 part of surfactant, 0.1-0.4 part of defoaming agent and 0.3-1.2 parts of cross-linking agent, wherein the bonding solvent type thermoplastic elastomer solution is a solution obtained by dissolving bonding solvent type thermoplastic elastomer solid in the solvent and having the mass concentration of 25%.
Further, the absorbent is at least one of flaky ferrosilicon powder, ferrosilicon aluminum powder, ferrosilicon chromium powder and ferrosilicon chromium nickel powder, and the Apparent Density (AD) of the flaky absorbent is 0.2-0.45.
The solvent-based thermoplastic elastomer for bonding is at least one of a thermoplastic polyurethane elastomer (TPU), a polyolefin thermoplastic elastomer (TPO), a styrene thermoplastic elastomer (SBC), a polyester thermoplastic elastomer (TPEE) and a polyamide thermoplastic elastomer (TPAE).
Further, the surfactant is at least one of modified phosphate ester polymer, epoxy resin and phenolic resin.
Further, the solvent is at least one of cyclohexanone (ANONE), Cycloheptane (Cycloheptane), dimethyl carbonate (DMC), N-Dimethylformamide (DMF) and propylene glycol methyl ether (PM).
Further, the defoaming agent is at least one of fluorocarbon modified organic silicon polymer, mineral oil defoaming agent and non-silicon polymer.
Further, the crosslinking agent is at least one of sulfur, dicumyl peroxide (DCP), bis-penta (2, 5-bis (tert-butylperoxy) -2, 5-dimethylhexane) and bis-tert-butylperoxyisopropyl benzene (BIPB).
The preparation method of the wave-absorbing material with high surface resistivity comprises the following steps:
(1) weighing an absorbent, a solvent and a surfactant, placing the absorbent, the solvent and the surfactant in a stirring and dispersing pot, stopping stirring after uniform stirring and dispersion, adding a bonding solvent type thermoplastic elastomer and a defoaming agent, adding a cross-linking agent after uniform stirring and dispersion, starting a vacuum pump, stirring and dispersing uniformly, and passing the slurry through a screen to remove impurities;
(2) coating the slurry obtained in the step (1) on a PET release film on a coating machine, wherein the coating and drying temperature is 60-150 ℃, and volatilizing the solvent to obtain a sheet-shaped coating or a roll-shaped coating with the thickness of 50-250 um;
(3) carrying out hot-pressing treatment on the flaky coating obtained in the step (2) for 1-10 minutes by adopting a vacuum-pumping flat vulcanizing machine under the conditions that the hot-pressing temperature is 150-; or the roll-shaped coating obtained in the step (2) is crosslinked and compacted by adopting a roll type continuous vulcanizing machine under the conditions that the hot pressing temperature is 170-210 ℃, the pressure is 2-10Mpa and the speed is 0.2-2 m/min, thus obtaining the high surface resistivity wave-absorbing material.
Further, the step (1) is specifically as follows: weighing 80-90 parts of flaky iron-silicon-aluminum powder absorbent, 70-100 parts of solvent and 0.2-0.8 part of surfactant, placing the materials in a stirring dispersion pot, setting the stirring speed to be 18 revolutions per minute, setting the temperature of the stirring pot to be 60 ℃, stirring for 2 hours, and stopping stirring; adding 50-70 parts of solvent type thermoplastic elastomer for bonding and 0.1-0.4 part of defoaming agent, setting the stirring speed to be 25 revolutions per minute, setting the dispersion speed to be 2500 revolutions per minute, setting the temperature of a stirring pot to be 60 ℃, stirring and dispersing for 2 hours, and stopping stirring; adding 0.3-1.2 parts of cross-linking agent, opening a vacuum pump, setting the stirring speed to be 25 r/min, setting the dispersion speed to be 1500 r/min, setting the temperature of a stirring pot to be 30 ℃, stirring and dispersing for 30 min, and passing the uniformly stirred and dispersed slurry through a screen to remove impurities.
Compared with the prior art, the invention has the advantages that: the invention discloses a high surface resistivity wave-absorbing material and a preparation method thereof, wherein the addition of a proper amount of a surfactant hardly influences or has little influence on the magnetic conductivity of the wave-absorbing material while the resistivity of the wave-absorbing material is improved.
Detailed Description
The present invention will be described in further detail with reference to examples.
Detailed description of the preferred embodiments
Example 1
A high surface resistivity wave-absorbing material is composed of the following raw materials in parts by weight: 85 parts of absorbent, 60 parts of solvent type thermoplastic elastomer solution for bonding, 85 parts of solvent, 0.42 part of surfactant, 0.3 part of defoaming agent and 0.6 part of cross-linking agent, wherein the preparation method comprises the following steps:
(1) weighing 85 parts of flaky ferrosilicon aluminum powder absorbent (AD of the powder is 0.35), 85 parts of DMF (dimethyl formamide) and DMC (dimethyl formamide) composite solvent and 0.42 part of modified phosphate polymer surfactant, and placing the mixture in a stirring dispersion pot; setting the stirring speed to be 18 revolutions per minute, setting the temperature of a stirring pot to be 60 ℃, stirring for 2 hours, stopping stirring, adding 60 parts of TPU solution (25 mass percent solution obtained by dissolving TPU solid in a composite solvent of DMF and DMC) and 0.3 part of fluorocarbon modified organic silicon polymer defoaming agent, setting the stirring speed to be 25 revolutions per minute, setting the dispersion speed to be 2500 revolutions per minute, setting the temperature of the stirring pot to be 60 ℃, and stirring and dispersing for 2 hours; stopping stirring, adding 0.6 part of bis-di-penta cross-linking agent, starting a vacuum pump, setting the stirring speed to be 25 revolutions per minute, setting the dispersion speed to be 1500 revolutions per minute, setting the temperature of a stirring pot to be 30 ℃, and stirring and dispersing for 30 minutes; passing the uniformly stirred and dispersed slurry through a screen to remove impurities;
(2) coating the slurry obtained in the step (1) on a PET release film on a coating machine, wherein the coating and drying temperature is 60-150 ℃, and volatilizing the solvent to obtain a roll-shaped coating with the thickness of 150 um;
(3) and (3) adopting a roller type continuous vulcanizing machine to crosslink and compact the roll-shaped coating obtained in the step (2) under the conditions that the hot pressing temperature is 180 ℃, the pressure is 8Mpa and the speed is 1 m/min, thus obtaining the wave-absorbing material with high surface resistivity. And (3) detecting the magnetic property and the surface resistance of the product, namely testing the magnetic permeability of the ring of the sheet punch F7X3mm obtained after hot pressing by using Agilent 4991B, and testing the surface resistivity of the ring by using a SIMCO ION ST-4 static measuring instrument.
Example 2
A high surface resistivity wave-absorbing material is composed of the following raw materials in parts by weight: 80 parts of absorbent, 50 parts of solvent type thermoplastic elastomer solution for bonding, 70 parts of solvent, 0.3 part of surfactant, 0.1 part of defoaming agent and 0.3 part of cross-linking agent, wherein the preparation method comprises the following steps:
(1) weighing 80 parts of flaky ferrosilicon aluminum powder absorbent (AD of the powder is 0.35), 70 parts of compound solvent of cycloheptanes and PM and 0.3 part of modified phosphate polymer surfactant, and placing the mixture in a stirring and dispersing pot; the stirring speed is set to be 18 r/min, the temperature of the stirring pot is 60 ℃, and the stirring is carried out for 2 hours; stopping stirring, adding 50 parts of SBC solution (25% by mass solution obtained by dissolving SBC solid in a composite solvent of cycloheptanes and PM) and 0.1 part of fluorocarbon modified organic silicon polymer defoaming agent, setting the stirring speed to 25 revolutions per minute, the dispersion speed to 2500 revolutions per minute, the temperature of a stirring pot to be 60 ℃, and stirring and dispersing for 2 hours; stopping stirring, adding 0.3 part of BIPB crosslinking agent, starting a vacuum pump, setting the stirring speed to be 25 revolutions per minute, setting the dispersion speed to be 1500 revolutions per minute, setting the temperature of a stirring pot to be 30 ℃, and stirring and dispersing for 30 minutes; passing the uniformly stirred and dispersed slurry through a screen to remove impurities;
(2) coating the slurry obtained in the step (1) on a PET release film on a coating machine, wherein the coating and drying temperature is 60-150 ℃, and volatilizing the solvent to obtain a sheet-shaped coating with the thickness of 50 um;
(3) and (3) carrying out hot-pressing treatment on the flaky coating obtained in the step (2) for 5 minutes by adopting a vacuum-pumping flat vulcanizing machine under the conditions that the hot-pressing temperature is 180 ℃ and the pressure is 20Mpa so as to ensure that the flaky coating is crosslinked and compact, thus obtaining the high-surface-resistivity wave-absorbing material. And (3) detecting the magnetic property and the surface resistance of the product, namely testing the magnetic permeability of the ring of the sheet punch F7X3mm obtained after hot pressing by using Agilent 4991B, and testing the surface resistivity of the ring by using a SIMCO ION ST-4 static measuring instrument.
Example 3
A high surface resistivity wave-absorbing material is composed of the following raw materials in parts by weight: 90 parts of absorbent, 70 parts of solvent type thermoplastic elastomer solution for bonding, 100 parts of solvent, 0.8 part of surfactant, 0.4 part of defoaming agent and 1.2 parts of cross-linking agent, wherein the preparation method comprises the following steps:
(1) weighing 90 parts of flaky ferrosilicon aluminum powder absorbent (0.35 part of powder), 100 parts of Cycloheptane (Cycloheptane) solvent and 0.8 part of modified phosphate polymer surfactant, and placing the materials in a stirring dispersion pot; the stirring speed is set to be 18 r/min, the temperature of the stirring pot is 60 ℃, and the stirring is carried out for 2 hours; stopping stirring, adding 70 parts of a polyolefin thermoplastic elastomer (TPO) solution (25 mass percent solution obtained by dissolving TPO solid in cycloheptane) and 0.4 part of a non-silicon polymer defoaming agent, setting the stirring speed to be 25 revolutions per minute, the dispersion speed to be 2500 revolutions per minute, the temperature of a stirring pot to be 60 ℃, and stirring and dispersing for 2 hours; stopping stirring, adding 1.2 parts of dicumyl peroxide (DCP) cross-linking agent, starting a vacuum pump, setting the stirring speed to be 25 revolutions per minute, setting the dispersion speed to be 1500 revolutions per minute, setting the temperature of a stirring pot to be 30 ℃, and stirring and dispersing for 30 minutes; passing the uniformly stirred and dispersed slurry through a screen to remove impurities;
(2) coating the slurry obtained in the step (1) on a PET release film on a coating machine, wherein the coating and drying temperature is 60-150 ℃, and volatilizing the solvent to obtain a sheet-shaped coating with the thickness of 250 um;
(3) and (3) carrying out hot pressing treatment on the flaky coating obtained in the step (2) for 10 minutes by adopting a vacuum-pumping flat vulcanizing machine under the conditions that the hot pressing temperature is 180 ℃ and the pressure is 30Mpa so as to ensure that the flaky coating is crosslinked and compact, thus obtaining the high-surface-resistivity wave-absorbing material. And (3) detecting the magnetic property and the surface resistance of the product, namely testing the magnetic permeability of the ring of the sheet punch F7X3mm obtained after hot pressing by using Agilent 4991B, and testing the surface resistivity of the ring by using a SIMCO ION ST-4 static measuring instrument.
In addition to the above-described embodiments, the solvent-based thermoplastic elastomer for bonding may be at least one of a polyolefin-based thermoplastic elastomer (TPO), a polyester-based thermoplastic elastomer (TPEE), and a polyamide-based thermoplastic elastomer (TPEE). The surfactant may also be a combination of a modified phosphate polymer, an epoxy resin, and a phenolic resin. The defoamer can also be a fluorocarbon modified silicone polymer, a mineral oil type defoamer, and a non-silicon polymer combination. The crosslinking agent may also be sulphur and dicumyl peroxide (DCP), and the absorbent powder may also have an AD value of any of 0.2, 0.45 and 0.2-0.45.
Example 4
The difference from example 1 is that an epoxy resin is used as the surfactant.
Example 5
The difference from example 1 is that a phenolic resin is used as the surfactant.
Comparative example 1
The difference from example 1 is that no surfactant is added.
Comparative example 2
The difference from example 1 is that the amount of the surfactant added is 0.84 part.
Comparative example 3
The difference from example 1 is that the amount of the surfactant added is 1 part.
Comparative example 4
The difference from example 1 is that the amount of the surfactant added is 2 parts.
Comparative example 5
The difference from example 1 is that the amount of the surfactant added is 0.18 part.
Comparative example 6
The difference from example 1 is that the amount of the surfactant added is 0.1 part.
Second, analysis of test results
1. Comparative examples with and without surfactant addition
And (3) detecting the magnetic property and the surface resistivity of the product, namely testing the magnetic permeability of the ring of the sheet punch F7X3 obtained after hot pressing by using Agilent 4991B, and testing the surface resistivity of the ring by using a SIMCO ION ST-4 static measuring instrument. Test results
Note: SIMCO ION ST-4 Electrostatic measuring apparatus 103-1013When it is less than 103Time also display 103。
From the results of the above examples and comparative examples, it can be seen that the surface resistivity of the wave-absorbing material can be significantly improved by adding the surfactant. The reason for analyzing that the surfactant enables the absorbent and the binder to be dispersed more uniformly, the wave-absorbing material after hot-pressing crosslinking is more compact and has fewer holes, the density increase of the embodiment and the comparative example 1 is just proved, the magnetic permeability can be increased, and the increased magnetic permeability counteracts the reduction of the magnetic permeability due to the non-magnetic phase of the surfactant.
The more the sheet-shaped absorbent in the wave-absorbing material is, the less the binder is, the higher the magnetic conductivity is, the lower the surface resistivity is, the less the sheet-shaped absorbent is, the more the binder is, the lower the magnetic conductivity is, the higher the surface resistivity is, the addition of the surfactant can improve the surface resistivity of the material, can cause certain reduction to the magnetic conductivity, and can properly reduce the addition amount of the binder to improve the magnetic conductivity. The surface resistivity of the wave-absorbing material can be improved by adjusting the addition amount of the surfactant, and the balance between the magnetic permeability and the surface resistivity is sought according to the application requirements of products so as to determine the addition amount of the surfactant.
The above description is not intended to limit the present invention, and the present invention is not limited to the above examples. Those skilled in the art should also realize that changes, modifications, additions and substitutions can be made without departing from the true spirit and scope of the invention.
Claims (9)
1. A high surface resistivity wave-absorbing material is characterized by comprising the following raw materials in parts by weight: 80-90 parts of absorbent, 50-70 parts of bonding solvent type thermoplastic elastomer, 70-100 parts of solvent, 0.2-0.8 part of surfactant, 0.1-0.4 part of defoaming agent and 0.3-1.2 parts of cross-linking agent, wherein the bonding solvent type thermoplastic elastomer solution is a solution obtained by dissolving bonding solvent type thermoplastic elastomer solid in the solvent and has the mass concentration of 25%.
2. The high surface resistivity wave-absorbing material of claim 1, wherein: the absorbent is at least one of flaky ferrosilicon powder, ferrosilicon aluminum powder, ferrosilicon chromium powder and ferrosilicon chromium nickel powder, and the loose packed density of the flaky absorbent is 0.2-0.45.
3. The high surface resistivity wave-absorbing material of claim 1, wherein: the solvent-type thermoplastic elastomer for bonding is at least one of thermoplastic polyurethane elastomer, polyolefin thermoplastic elastomer, styrene thermoplastic elastomer, polyester thermoplastic elastomer and polyamide thermoplastic elastomer.
4. The high surface resistivity wave-absorbing material of claim 1, wherein: the surfactant is at least one of modified phosphate ester polymer, epoxy resin and phenolic resin.
5. The high surface resistivity wave-absorbing material of claim 1, wherein: the solvent is at least one of cyclohexanone, cycloheptane, dimethyl carbonate, N-dimethylformamide and propylene glycol methyl ether.
6. The high surface resistivity wave-absorbing material of claim 1, wherein: the defoaming agent is at least one of fluorocarbon modified organic silicon polymer, mineral oil defoaming agent and non-silicon polymer.
7. The high surface resistivity wave-absorbing material of claim 1, wherein: the cross-linking agent is at least one of sulfur, dicumyl peroxide, bis-penta-and bis-tert-butylperoxyisopropyl benzene.
8. A method for preparing the high surface resistivity wave-absorbing material in any one of claims 1 to 7, which is characterized by comprising the following steps:
(1) weighing an absorbent, a solvent and a surfactant, placing the absorbent, the solvent and the surfactant in a stirring and dispersing pot, stopping stirring after uniform stirring and dispersion, adding a bonding solvent type thermoplastic elastomer and a defoaming agent, adding a cross-linking agent after uniform stirring and dispersion, starting a vacuum pump, stirring and dispersing uniformly, and passing the slurry through a screen to remove impurities;
(2) coating the slurry obtained in the step (1) on a PET release film on a coating machine, wherein the coating and drying temperature is 60-150 ℃, and volatilizing the solvent to obtain a sheet-shaped coating or a roll-shaped coating with the thickness of 50-250 um;
(3) carrying out hot-pressing treatment on the flaky coating obtained in the step (2) for 1-10 minutes by adopting a vacuum-pumping flat vulcanizing machine under the conditions that the hot-pressing temperature is 150-; or the roll-shaped coating obtained in the step (2) is crosslinked and compacted by adopting a roll type continuous vulcanizing machine under the conditions that the hot pressing temperature is 170-210 ℃, the pressure is 2-10Mpa and the speed is 0.2-2 m/min, thus obtaining the high surface resistivity wave-absorbing material.
9. The method for preparing the wave-absorbing material with high surface resistivity according to claim 8, wherein the step (1) is as follows: weighing 80-90 parts of flaky iron-silicon-aluminum powder absorbent, 70-100 parts of solvent and 0.2-0.8 part of surfactant, placing the materials in a stirring dispersion pot, setting the stirring speed to be 18 revolutions per minute, setting the temperature of the stirring pot to be 60 ℃, stirring for 2 hours, and stopping stirring; adding 50-70 parts of solvent type thermoplastic elastomer for bonding and 0.1-0.4 part of defoaming agent, setting the stirring speed to be 25 revolutions per minute, setting the dispersion speed to be 2500 revolutions per minute, setting the temperature of a stirring pot to be 60 ℃, stirring and dispersing for 2 hours, and stopping stirring; adding 0.3-1.2 parts of cross-linking agent, opening a vacuum pump, setting the stirring speed to be 25 r/min, setting the dispersion speed to be 1500 r/min, setting the temperature of a stirring pot to be 30 ℃, stirring and dispersing for 30 min, and passing the uniformly stirred and dispersed slurry through a screen to remove impurities.
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