CN111002674B - Composite electromagnetic shielding material and preparation method thereof - Google Patents
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- B29C43/22—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of indefinite length
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- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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Abstract
The invention belongs to the technical field of shielding materials, and discloses a composite electromagnetic shielding material and a preparation method thereof. The composite electromagnetic shielding material comprises a polymer, alloy powder, polyaniline, graphene, an organic solvent and an adhesive, wherein the polymer is one of polyethylene, polypropylene, polystyrene and polyamide. The composite electromagnetic shielding material provided by the invention enhances the electromagnetic shielding performance by combining the high-conductivity material and the high-eddy-current-effect material, and the prepared composite electromagnetic shielding material has a good electromagnetic shielding effect on electromagnetic waves in a wide frequency band, is light and has good mechanical properties.
Description
Technical Field
The invention relates to the technical field of shielding materials, in particular to a composite electromagnetic shielding material and a preparation method thereof.
Background
In recent years, with the continuous development of electronic communication and industrial civilization, electromagnetic interference is becoming more and more serious due to the popularization of electronic equipment and wireless communication systems, and the normal operation of electronic equipment systems is greatly influenced. In addition, more and more electronic and electrical devices and communication systems are rapidly changed, so that people can quickly and conveniently transmit information and serious electromagnetic pollution is caused, the generated electromagnetic waves are seriously harmful to the working and living environment of people, the ecological environment required by the health and sustainable development of people is seriously influenced, and huge losses are caused to the country. In order to reduce the harm caused by electromagnetic pollution, research on novel electromagnetic shielding composite materials with higher performance has become an important direction for technical development.
Currently, the commonly used electromagnetic shielding material is a blend of conductive filler and resin, such as gold, silver, copper or graphite, which is mixed with a polymer to improve the conductivity thereof, thereby improving the electromagnetic shielding effect, but the polymer matrix has better electrical insulation property and has limited effect of improving the electromagnetic shielding performance. In addition, researchers also blend soft magnetic materials and polymers to prepare electromagnetic shielding materials, but the electromagnetic shielding effect of the composite material is not ideal enough, and meanwhile, the increase of the filling amount can cause processing difficulty and influence the mechanical properties of the material. In addition, researchers mix and press the granular pore-forming agent and the biomass material for molding, and prepare the shielding material with the low-density and wide-frequency porous composite structure through sintering treatment, but the filling material prepared by the method has limited shielding effect, weak chemical corrosion resistance and poor mechanical property.
Disclosure of Invention
The invention provides a composite electromagnetic shielding material and a preparation method thereof in order to overcome the defects of the background technology. The composite electromagnetic shielding material provided by the invention enhances the electromagnetic shielding performance by combining the high-conductivity material and the high-eddy-current-effect material, and the prepared composite electromagnetic shielding material has a good electromagnetic shielding effect on electromagnetic waves in a wide frequency band, is light and has good mechanical properties.
In order to achieve the purpose of the invention, the composite electromagnetic shielding material comprises a polymer, alloy powder, polyaniline, graphene, an organic solvent and an adhesive, wherein the polymer is one of polyethylene, polypropylene, polystyrene and polyamide.
Further, the mass ratio of the polyaniline to the organic solvent is 1: (5-20), wherein the mass ratio of the graphene to the organic solvent is 1: (8-20), uniformly stirring the polyaniline and the graphene, dispersing the polyaniline and the graphene in an organic solvent to obtain a mixed solution, and drying the mixed solution at the temperature of 60-85 ℃ to obtain mixed powder.
Further, the mass ratio of the polyaniline to the polymer is 1: (2-18); the mass ratio of the graphene to the polymer is 1: (2-25).
Further, the mass ratio of the alloy powder to the adhesive is (2-12): 1.
further, the polyaniline is conductive polyaniline, and the particle size range is 2-5 mu m; the particle size range of the graphene is 7-12 mu m.
Further, the organic solvent is one or a mixture of ethanol, propanol, butanol and xylene.
Further, the alloy powder is a mixture of one or more of Fe-Ni-Mo, Fe-Si-Cr and Fe-Si-Al.
Further, the adhesive is one or a mixture of polyvinyl butyral, waterborne polyurethane and phenolic-butyronitrile.
On the basis of the technical scheme, the invention also provides a preparation method of the composite electromagnetic shielding material, which comprises the following steps:
(1) stirring polyaniline and graphene uniformly, dispersing the polyaniline and the graphene in an organic solvent to obtain a mixed solution, and drying the mixed solution at 60-85 ℃ to obtain mixed powder;
(2) mixing a polymer and the mixed powder in the step (1) in a ratio of 2-7: 1, mixing in an internal mixer, mixing the mixed mixture, and calendering to obtain a polymer film;
(3) dispersing 50-100 parts by weight of alloy powder into 25-100 parts by weight of organic solvent, adding 5-15 parts by weight of adhesive, uniformly stirring to obtain a mixed solution, and obtaining an alloy powder film by a tape casting process;
(4) and laminating the polymer film and the alloy powder film, and rolling to obtain the composite electromagnetic shielding material.
Further, the mixture blended in the step (2) is mixed under 30-80 MPa, and the rolling temperature in the step (4) is 150-270 ℃.
Compared with the prior art, the invention has the following advantages:
(1) according to the invention, high-conductivity polyaniline and graphene are compounded to obtain the shielding material with a good reflection effect on an electromagnetic field, so that the shielding effect of the material is enhanced;
(2) according to the invention, the high-frequency high-permeability alloy powder is uniformly dispersed in the organic adhesive, so that the eddy current effect is enhanced, and the high-frequency electromagnetic shielding effect is increased;
(3) the method has the advantages of easily obtained raw materials, simple steps, convenient operation, short forming time, adjustable required thickness according to requirements, better electromagnetic shielding effect of the obtained composite material and lower density.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention. It is to be understood that the following description is only illustrative of the present invention and is not to be construed as limiting the present invention.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
Example 1
Adding 5g of conductive polyaniline and 2.5g of graphene into 50mL of butanol, and ultrasonically stirring and dispersing for 10 min. Then, the mixture was dried in a vacuum oven at 75 ℃ for 12 hours or more. The dried powder was added to an internal mixer together with 36g of polypropylene and internally mixed for 3 hours at 160 ℃ and a frequency of 30 Hz. The mixture after internal mixing was mixed at a roll speed of 1.5m/min and a temperature of 156 ℃. And then calendering the mixed material, adjusting the roll temperature to 160 ℃, and controlling the roll speed to be 1m/min to obtain the polymer film.
Weighing 24g of iron-silicon-aluminum alloy powder, adding into 35g of xylene solvent, adding 3g of phenolic aldehyde-butyronitrile, mixing to obtain slurry, introducing the mixed slurry into a scraper groove, and carrying out tape casting at a tape running speed of 1m/min to obtain an alloy powder film.
Laminating the polypropylene film and the alloy powder film, and rolling at the roll temperature of 160 ℃ and the roll speed of 1.8m/min to obtain the 0.3mm electromagnetic shielding composite material. The tensile strength of the electromagnetic shielding composite material sample is 30MPa, and the electromagnetic shielding efficiency value is 25dB at 0.5 GHz-2 GHz.
Example 2
Adding 6g of conductive polyaniline and 3.5g of graphene into 50mL of butanol, and ultrasonically stirring and dispersing for 10 min. Then, the mixture was dried in a vacuum oven at 75 ℃ for 12 hours or more. The dried powder was added to an internal mixer together with 36g of polypropylene and internally mixed for 3 hours at a temperature of 162 ℃ and a frequency of 30 Hz. The mixture after internal mixing was mixed at a roll speed of 1.5m/min and a temperature of 156 ℃. And then calendering the mixed material, adjusting the roll temperature to 160 ℃, and controlling the roll speed to be 1m/min to obtain the polymer film.
Weighing 24g of iron-silicon-aluminum alloy powder, adding into 35g of xylene solvent, adding 3g of phenolic aldehyde-butyronitrile, mixing to obtain slurry, introducing the mixed slurry into a scraper groove, and carrying out tape casting at a tape running speed of 1m/min to obtain an alloy powder film.
Laminating the polypropylene film and the alloy powder film, and rolling at the roll temperature of 160 ℃ and the roll speed of 1.8m/min to obtain the 0.3mm electromagnetic shielding composite material. The tensile strength of the electromagnetic shielding composite material sample is 23MPa, and the electromagnetic shielding efficiency value is 30dB at 0.5 GHz-2 GHz.
Example 3
Adding 3g of conductive polyaniline and 3g of graphene into 50mL of butanol, and ultrasonically stirring and dispersing for 10 min. Then, the mixture was dried in a vacuum oven at 75 ℃ for 12 hours or more. The dried powder was added to an internal mixer together with 36g of polypropylene and internally mixed for 3 hours at 160 ℃ and a frequency of 30 Hz. The mixture after internal mixing was mixed at a roll speed of 1m/min and a temperature of 156 ℃. And then calendering the mixed material, adjusting the roll temperature to 160 ℃, and controlling the roll speed to 1.5m/min to obtain the polymer film.
Weighing 24g of iron-silicon-aluminum alloy powder, adding into 35g of xylene solvent, adding 3g of phenolic aldehyde-butyronitrile, mixing to obtain slurry, introducing the mixed slurry into a scraper groove, and carrying out tape casting at a tape running speed of 1m/min to obtain an alloy powder film.
Laminating the polypropylene film and the alloy powder film, and rolling at the roll temperature of 160 ℃ and the roll speed of 1.8m/min to obtain the 0.3mm electromagnetic shielding composite material. The tensile strength of the electromagnetic shielding composite material sample is 35MPa, and the electromagnetic shielding efficiency value is 18dB at 0.5 GHz-2 GHz.
Example 4
Adding 5g of conductive polyaniline and 3g of graphene into 50mL of butanol, and ultrasonically stirring and dispersing for 10 min. Then, the mixture was dried in a vacuum oven at 75 ℃ for 12 hours or more. The dried powder was added to an internal mixer together with 36g of polypropylene and internally mixed for 3 hours at 160 ℃ and a frequency of 25 Hz. The mixture after internal mixing was mixed at a roll speed of 1.6m/min and a temperature of 156 ℃. And then calendering the mixed material, adjusting the roll temperature to 160 ℃, and controlling the roll speed to be 1m/min to obtain the polymer film.
Weighing 30g of iron-silicon-aluminum alloy powder, adding into 35g of xylene solvent, adding 3g of phenolic aldehyde-butyronitrile, mixing to obtain slurry, introducing the mixed slurry into a scraper groove, and carrying out tape casting at a tape running speed of 1.2m/min to obtain an alloy powder film.
Laminating the polypropylene film and the alloy powder film, and rolling at the roll temperature of 160 ℃ and the roll speed of 1.5m/min to obtain the 0.3mm electromagnetic shielding composite material. The tensile strength of the electromagnetic shielding composite material sample is 20MPa, and the electromagnetic shielding efficiency value is 36dB at 0.5 GHz-2 GHz.
Example 5
Adding 3g of conductive polyaniline and 5g of graphene into 50mL of butanol, and ultrasonically stirring and dispersing for 10 min. Then, the mixture was dried in a vacuum oven at 75 ℃ for 12 hours or more. The dried powder was added to an internal mixer together with 36g of polypropylene and internally mixed for 3 hours at 160 ℃ and a frequency of 28 Hz. The mixture after internal mixing was mixed at a roll speed of 1.5m/min and a temperature of 156 ℃. And then calendering the mixed material, adjusting the roll temperature to 160 ℃, and controlling the roll speed to be 1m/min to obtain the polymer film.
Weighing 18g of iron-silicon-aluminum alloy powder, adding into 35g of xylene solvent, adding 6g of phenolic aldehyde-butyronitrile, mixing to obtain slurry, introducing the mixed slurry into a scraper groove, and carrying out tape casting at a tape running speed of 1m/min to obtain an alloy powder film.
Laminating the polypropylene film and the alloy powder film, and rolling at the roll temperature of 160 ℃ and the roll speed of 1.8m/min to obtain the 0.3mm electromagnetic shielding composite material. The tensile strength of the electromagnetic shielding composite material sample is 30MPa, and the electromagnetic shielding efficiency value is 28dB at 0.5 GHz-2 GHz.
Example 6
Adding 4g of conductive polyaniline and 2.5g of graphene into 50mL of butanol, and ultrasonically stirring and dispersing for 10 min. Then, the mixture was dried in a vacuum oven at 75 ℃ for 12 hours or more. The dried powder was added to an internal mixer together with 40g of polypropylene and internally mixed for 3 hours at 160 ℃ and a frequency of 22 Hz. The mixture after internal mixing was mixed at a roll speed of 1.5m/min and a temperature of 158 ℃. And then calendering the mixed material, adjusting the roll temperature to 160 ℃, and controlling the roll speed to be 1m/min to obtain the polymer film.
Weighing 24g of iron-silicon-aluminum alloy powder, adding into 35g of xylene solvent, adding 3g of phenolic aldehyde-butyronitrile, mixing to obtain slurry, introducing the mixed slurry into a scraper groove, and carrying out tape casting at a tape running speed of 1m/min to obtain an alloy powder film.
Laminating the polypropylene film and the alloy powder film, and rolling at the roll temperature of 160 ℃ and the roll speed of 1.8m/min to obtain the 0.3mm electromagnetic shielding composite material. The tensile strength of the electromagnetic shielding composite material sample is 42MPa, and the electromagnetic shielding efficiency value is 21dB at 0.5 GHz-2 GHz.
Example 7
Adding 5g of conductive polyaniline and 2.5g of graphene into 50mL of butanol, and ultrasonically stirring and dispersing for 10 min. Then, the mixture was dried in a vacuum oven at 75 ℃ for 12 hours or more. The dried powder was added to an internal mixer together with 25g of polypropylene and internally mixed for 3 hours at 160 ℃ and a frequency of 40 Hz. The mixture after internal mixing was mixed at a roll speed of 1.5m/min and a temperature of 156 ℃. And then calendering the mixed material, adjusting the roll temperature to 160 ℃, and controlling the roll speed to be 1m/min to obtain the polymer film.
Weighing 36g of iron-silicon-aluminum alloy powder, adding into 35g of xylene solvent, adding 4g of phenolic aldehyde-butyronitrile, mixing to obtain slurry, introducing the mixed slurry into a scraper groove, and carrying out tape casting at a tape running speed of 1m/min to obtain an alloy powder film.
Laminating the polypropylene film and the alloy powder film, and rolling at the roll temperature of 160 ℃ and the roll speed of 1.8m/min to obtain the 0.3mm electromagnetic shielding composite material. The tensile strength of the electromagnetic shielding composite material sample is 17MPa, and the electromagnetic shielding efficiency value is 41dB at 0.5 GHz-2 GHz.
Example 8
Adding 5g of conductive polyaniline and 3.5g of graphene into 50mL of butanol, and ultrasonically stirring and dispersing for 10 min. Then, the mixture was dried in a vacuum oven at 75 ℃ for 12 hours or more. The dried powder was added to an internal mixer together with 50g of polypropylene and internally mixed for 3 hours at 160 ℃ and a frequency of 30 Hz. The mixture after internal mixing was mixed at a roll speed of 1.5m/min and a temperature of 156 ℃. And then calendering the mixed material, adjusting the roll temperature to 160 ℃, and controlling the roll speed to be 1m/min to obtain the polymer film.
Weighing 21g of iron-silicon-aluminum alloy powder, adding into 35g of xylene solvent, adding 3g of phenolic aldehyde-butyronitrile, mixing to obtain slurry, introducing the mixed slurry into a scraper groove, and carrying out tape casting at a tape running speed of 1m/min to obtain an alloy powder film.
Laminating the polypropylene film and the alloy powder film, and rolling at the roll temperature of 160 ℃ and the roll speed of 1.8m/min to obtain the 0.3mm electromagnetic shielding composite material. The tensile strength of the electromagnetic shielding composite material sample is 45MPa, and the electromagnetic shielding efficiency value is 27dB at 0.5 GHz-2 GHz.
Example 9
Adding 6g of conductive polyaniline and 5g of graphene into 50mL of butanol, and ultrasonically stirring and dispersing for 10 min. Then, the mixture was dried in a vacuum oven at 75 ℃ for 12 hours or more. The dried powder was added to an internal mixer together with 40g of polypropylene and internally mixed for 3 hours at 160 ℃ and a frequency of 30 Hz. The mixture after internal mixing was mixed at a roll speed of 1.5m/min and a temperature of 156 ℃. And then calendering the mixed material, adjusting the roll temperature to 160 ℃, and controlling the roll speed to be 1m/min to obtain the polymer film.
Weighing 24g of iron-silicon-aluminum alloy powder, adding into 35g of xylene solvent, adding 6g of phenolic aldehyde-butyronitrile, mixing to obtain slurry, introducing the mixed slurry into a scraper groove, and carrying out tape casting at a tape running speed of 1m/min to obtain an alloy powder film.
Laminating the polypropylene film and the alloy powder film, and rolling at the roll temperature of 160 ℃ and the roll speed of 1.8m/min to obtain the 0.3mm electromagnetic shielding composite material. The tensile strength of the electromagnetic shielding composite material sample is 33MPa, and the electromagnetic shielding efficiency value is 28dB at 0.5 GHz-2 GHz.
Example 10
Adding 7.2g of conductive polyaniline and 4g of graphene into 50mL of butanol, and ultrasonically stirring and dispersing for 10 min. Then, the mixture was dried in a vacuum oven at 75 ℃ for 12 hours or more. The dried powder was added to an internal mixer together with 36g of polypropylene and internally mixed for 3 hours at 160 ℃ and a frequency of 30 Hz. The mixture after internal mixing was mixed at a roll speed of 1.5m/min and a temperature of 156 ℃. And then calendering the mixed material, adjusting the roll temperature to 160 ℃, and controlling the roll speed to be 1m/min to obtain the polymer film.
Weighing 27g of iron-silicon-aluminum alloy powder, adding into 35g of xylene solvent, adding 3g of phenolic aldehyde-butyronitrile, mixing to obtain slurry, introducing the mixed slurry into a scraper groove, and carrying out tape casting at a tape running speed of 1m/min to obtain an alloy powder film.
Laminating the polypropylene film and the alloy powder film, and rolling at the roll temperature of 160 ℃ and the roll speed of 1.8m/min to obtain the 0.3mm electromagnetic shielding composite material. The tensile strength of the electromagnetic shielding composite material sample is 27MPa, and the electromagnetic shielding efficiency value is 52dB at 0.5 GHz-2 GHz.
It will be understood by those skilled in the art that the foregoing is only exemplary of the present invention, and is not intended to limit the invention, which is intended to cover any variations, equivalents, or improvements therein, which fall within the spirit and scope of the invention.
Claims (7)
1. The composite electromagnetic shielding material is characterized by comprising a polymer, alloy powder, polyaniline, graphene, an organic solvent and an adhesive, wherein the polymer is one of polyethylene, polypropylene, polystyrene and polyamide;
the mass ratio of the polyaniline to the organic solvent is 1: (5-20), wherein the mass ratio of the graphene to the organic solvent is 1: (8-20), uniformly stirring the polyaniline and the graphene, dispersing the polyaniline and the graphene in an organic solvent to obtain a mixed solution, and drying the mixed solution at the temperature of 60-85 ℃ to obtain mixed powder;
the mass ratio of the polyaniline to the polymer is 1: (2-18); the mass ratio of the graphene to the polymer is 1: (2-25);
the composite electromagnetic shielding material is prepared by the following method, comprising the following steps:
(1) stirring polyaniline and graphene uniformly, dispersing the polyaniline and the graphene in an organic solvent to obtain a mixed solution, and drying the mixed solution at 60-85 ℃ to obtain mixed powder;
(2) mixing a polymer and the mixed powder in the step (1) in a ratio of 2-7: 1, mixing in an internal mixer, mixing the mixed mixture, and calendering to obtain a polymer film;
(3) dispersing 50-100 parts by weight of alloy powder into 25-100 parts by weight of organic solvent, adding 5-15 parts by weight of adhesive, uniformly stirring to obtain a mixed solution, and obtaining an alloy powder film by a tape casting process;
(4) and laminating the polymer film and the alloy powder film, and rolling to obtain the composite electromagnetic shielding material.
2. The composite electromagnetic shielding material according to claim 1, wherein the mass ratio of the alloy powder to the binder is (2-12): 1.
3. the composite electromagnetic shielding material of claim 1, wherein the polyaniline is conductive polyaniline, and the particle size ranges from 2 to 5 μm; the particle size range of the graphene is 7-12 mu m.
4. The composite electromagnetic shielding material of claim 1, wherein the organic solvent is a mixture of one or more of ethanol, propanol, butanol, and xylene.
5. The composite electromagnetic shielding material of claim 1, wherein the alloy powder is a mixture of one or more of Fe-Ni-Mo, Fe-Si-Cr, and Fe-Si-Al.
6. The composite electromagnetic shielding material of claim 1, wherein the adhesive is one or more of polyvinyl butyral, aqueous polyurethane, and phenol-butadiene-acrylonitrile.
7. The composite electromagnetic shielding material of claim 1, wherein the mixture blended in step (2) is mixed under 30-80 MPa, and the rolling temperature in step (4) is 150-270 ℃.
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| CN105602145A (en) * | 2016-01-28 | 2016-05-25 | 西安科技大学 | Polymer-graphene-polyaniline electromagnetic shielding composite and preparing method thereof |
| CN105820499A (en) * | 2016-05-25 | 2016-08-03 | 贾涵楠 | Polyaniline composite conductive plastic |
| CN107912012A (en) * | 2017-11-29 | 2018-04-13 | 横店集团东磁股份有限公司 | A kind of electromagnetic wave shielding/absorption composite paster and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105602145A (en) * | 2016-01-28 | 2016-05-25 | 西安科技大学 | Polymer-graphene-polyaniline electromagnetic shielding composite and preparing method thereof |
| CN105820499A (en) * | 2016-05-25 | 2016-08-03 | 贾涵楠 | Polyaniline composite conductive plastic |
| CN107912012A (en) * | 2017-11-29 | 2018-04-13 | 横店集团东磁股份有限公司 | A kind of electromagnetic wave shielding/absorption composite paster and preparation method thereof |
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