CN110172260B - Light electromagnetic shielding sealing material and preparation method and application thereof - Google Patents
Light electromagnetic shielding sealing material and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a light electromagnetic shielding sealing material, which is prepared from the following raw materials: expanded polymer microspheres, carbon materials; wherein the mass ratio of the polymer expanded microspheres to the carbon material is (64-2): 1. further, the raw material also comprises a coupling agent, and the mass of the coupling agent is 1-2% of the total mass of the polymer expanded microspheres and the carbon material, and is preferably 2%. The light electromagnetic shielding sealing material has the advantages of small density, excellent electric conduction and electromagnetic shielding performance and the like, and is very suitable to be used as an electric conduction material and an electromagnetic shielding material. Moreover, the preparation method of the light electromagnetic shielding sealing material is simple and convenient, low in energy consumption, high in production efficiency and quite good in industrialization prospect.
Description
Technical Field
The invention belongs to the field of high-molecular electromagnetic shielding materials, and particularly relates to a light electromagnetic shielding sealing material, and a preparation method and application thereof.
Background
The emergence of electromagnetic waves has greatly promoted social progress, and the development of modern electronic information technology is inseparable from electromagnetic waves. However, the widespread use of electronic devices also causes a great deal of electromagnetic leakage and pollution, which not only interferes with the normal operation of electronic components and causes equipment failure, but also causes environmental pollution, harms the health of people and even more seriously causes information leakage.
The electromagnetic leakage of the electronic device is caused by the failure to obtain a good shield seal at the joints of the respective elements constituting the device, the opening and closing gaps of the housing, and the like. Thus, there is a need to explore and develop shielding materials with certain forms to meet the sealing requirements under different circumstances.
As a material capable of satisfying the shielding sealing, it should have characteristics of compressibility, electric conductivity or magnetic conductivity, electromagnetic shielding or absorption, and the like. Rubber composite materials containing conductive or magnetic fillers are often used in various sealing fields, and the composite materials are prepared by taking elastic materials such as polyurethane, natural rubber, butyl rubber, ethylene propylene diene monomer rubber and the like as matrixes, adding fillers such as carbon nanotubes, graphene, carbon fibers, metal-plated fibers and the like, and processing the fillers by a specific method. In order to obtain the required electromagnetic shielding performance, the content of the filler in the electromagnetic sealing material is high, and the preparation cost is high. In order to obtain excellent electromagnetic shielding effect at a reduced cost, research attempts have been made to further improve the conductive electromagnetic shielding performance by performing foaming operation (ACS Applied Materials & Interfaces, 2011, 3: 918-. There have also been studies to coat a metal nano-film on the skeleton of a flexible open-cell foam (chinese patent ZL201410414514.1, US 6309742B1), so that excellent shielding effect can be obtained at a lower metal content and compressibility is also obtained. However, the chemical plating or electroplating technology used in the method can generate a large amount of heavy metal pollution in the preparation process, and the metal on the foam framework has the defects of non-corrosion resistance and the like. Research shows that the continuous conductive network formed inside the composite material can raise the electromagnetic shielding performance of the material. Researchers have developed insulation structural composites, i.e., forming a continuous filler-rich phase and a resin matrix phase within the composite. For example, DX Yan et al (Advanced Functional Materials, 2015, 25: 559-566) prepared the electromagnetic shielding composite material with the isolation structure by loading graphene on the surface of polystyrene resin microspheres and applying high pressure to the surface of the polystyrene resin microspheres. However, the method requires extremely high pressure to bond the resin together, and the obtained material has low mechanical strength and is not suitable for industrial production and application.
Disclosure of Invention
In order to obtain a simple method for preparing a sealing material with excellent electromagnetic properties, the inventors of the present application have surprisingly obtained a lightweight electromagnetic shielding sealing material through a great deal of research and practice, and have achieved technical effects that are not expected by those skilled in the art.
The invention aims to provide a light electromagnetic shielding sealing material, which is characterized in that: the preparation is prepared from the following raw materials:
expanded polymer microspheres, carbon materials;
wherein the mass ratio of the polymer expanded microspheres to the carbon material is (64-2): 1.
further, the raw material also comprises a coupling agent, and the mass of the coupling agent is 1-2% of the total mass of the polymer expanded microspheres and the carbon material, and is preferably 2%.
Further, the mass ratio of the expanded polymer microspheres to the carbon material is (16-2): 1, preferably 2: 1.
furthermore, the polymer expanded microsphere is a hollow sphere which takes a thermoplastic polymer as a shell and takes volatile organic compounds as a core;
preferably, the polymer expanded microspheres are selected from Akzo Nobel EXPANCELTM 031DU40，AkzoNobel EXPANCELTM051DU40, Advancell EHM303, Advancell EM 501.
Further, the carbon material is selected from one or more of graphene, carbon nanotubes, conductive carbon black and carbon nanofibers, preferably, the graphene is mechanically exfoliated graphene, and the carbon nanotubes are multi-walled carbon nanotubes.
Further, the coupling agent is selected from: silane coupling agent, titanate coupling agent, aluminate coupling agent and borate coupling agent.
Further, the light electromagnetic shielding sealing material is composed of a hollow polymer spherical shell and a carbon material sandwiched between the spherical shells.
The invention also provides a method for preparing the light electromagnetic shielding sealing material, which comprises the following steps:
i. taking raw materials, and uniformly dispersing to obtain intermediate powder;
and ii, adding the intermediate powder obtained in the step i into a mold cavity, and obtaining the light electromagnetic shielding sealing material under the conditions of temperature rise and pressure.
Further, in step i, the uniform dispersion mode is as follows: taking raw materials, adding a solvent, mechanically stirring or ultrasonically dispersing, then filtering, and taking a solid; or, taking the raw materials, and mechanically stirring;
the solvent is selected from an alcohol solvent or an alcohol aqueous solution;
and/or in step ii, the temperature rise and pressure increase conditions are as follows: the temperature is 140-300 ℃, the pressure is the lowest pressure of 15MPa which enables the mold cavity to keep a closed state, and the holding time is 3-60 min; preferably, the temperature is 160-250 ℃, the pressure is 2-10 MPa, and the holding time is 5-30 min.
The invention also provides application of the light electromagnetic shielding sealing material as a conductive material and/or an electromagnetic shielding material.
In the invention, the forming process of the light electromagnetic shielding sealing material comprises the following steps: at high temperature, the spherical shell of the polymer expanded microsphere is softened, the internal low-boiling-point organic matter volatilizes to expand the microsphere, and the carbon material is extruded in the middle of the spherical shell of the polymer. In addition, since the carbon material is randomly dispersed, the polymer shells are pressed against each other to be bonded together where there is no carbon material between the spheres, so that the resulting material has a certain interfacial bonding strength.
The invention has the following beneficial effects:
(1) the polymer is expanded to be a matrix, and the carbon material is clamped between the expanded polymer spherical shells under the driving of an expansion force, so that the preparation method is extremely simple, easy to realize and very suitable for large-scale application;
(2) the light electromagnetic shielding sealing material prepared by the invention can obtain excellent shielding effect under the condition of less carbon material consumption, and the obtained material has low comprehensive cost;
(3) the electromagnetic shielding sealing material prepared by the invention has light weight, and the lowest density can reach 0.3g/cm 3;
(4) the electromagnetic shielding sealing material prepared by the invention has excellent conductivity, and the lowest resistivity can reach 0.01 omega cm;
(5) the electromagnetic shielding sealing material prepared by the invention has excellent electromagnetic shielding performance, and the highest electromagnetic shielding performance in the range of 0.05-20 GHz can reach 120 dB.
The light electromagnetic shielding sealing material has the advantages of small density, excellent conductivity and electromagnetic shielding performance, adjustable performance and the like, is very suitable for being used as a conductive material and/or an electromagnetic shielding material, and has the advantages of simple and convenient preparation method, environmental protection, low energy consumption, high production efficiency and very good industrialization prospect.
Obviously, many modifications, substitutions, and variations are possible in light of the above teachings of the invention, without departing from the basic technical spirit of the invention, as defined by the following claims.
The present invention will be described in further detail with reference to the following examples. This should not be understood as limiting the scope of the above-described subject matter of the present invention to the following examples. All the technologies realized based on the above contents of the present invention belong to the scope of the present invention.
Drawings
FIG. 1 is a graph showing the electromagnetic shielding performance of the lightweight electromagnetic shielding sealing material numbered 1-5 to 1-9 in example 1 of the present invention.
Detailed Description
The raw materials and equipment used in the examples of the present invention can be obtained by purchasing commercially available products.
First, the main raw materials
1. Polymer expanded microspheres: akzo Nobel EXPANCELTM 031DU40，051DU40；Advancell EHM303，EM 501。
2. Carbon material: mechanically exfoliated graphene (HE01, dodecene carbon technology); multi-walled carbon nanotubes (TNFN-8, institute of organic chemistry, national institute of sciences); conductive carbon black (angongdelong chemical); carbon nanofibers (beijing delco island gold technology).
3. Coupling agent: silane coupling agent KH550, titanate coupling agent YB-201, aluminate coupling agent AD-50 and borate coupling agent LD-100P.
Second, performance test
1. The resistance of the resulting wafer sample was tested using a multimeter and the resistivity p was calculated according to the following formula:
r is resistance; r is the radius and L is the thickness.
2. According to the principle of a coaxial method, an KEYSIGHT PNA-X N5247A vector network analyzer is adopted to measure the electromagnetic shielding effectiveness of a wafer sample, the scanning frequency range is 0.05-20 GHz, the diameter of the sample is 11mm, and the thickness of the sample is 2 mm.
3. The apparent density of the sample is tested by a weighing method;
4. an INSTRON 4302 type universal material testing machine is adopted to test the compression performance of a cylindrical sample (phi 30 multiplied by 15mm), a sensor is 30KN, the testing speed is 2mm/min, and the mechanical performance of the sample is measured by the compression strength when the strain is 10%.
Example 1
According to the formula shown in table 1, taking polymer expanded microspheres 031DU40, mechanically stripping graphene, adding 20g of ethanol/water mixture with the concentration of 75 vol%, adding coupling agent KH550 according to 2% of the total mass of the microspheres and graphene, and mechanically stirring to uniformly disperse the mixture. And then filtering the mixture by using a funnel, taking the solid, and then transferring the solid to a blast oven to dry the solid at the temperature of 60 ℃ to obtain the microsphere-graphene composite powder.
Adding a certain amount of microsphere-graphene composite powder into a mold cavity with the diameter of 30mm and the thickness of 15mm, keeping the temperature at 160 ℃ and the pressure of 2MPa for 30min, stopping heating, removing the pressure after the temperature is reduced to room temperature, and opening the mold to obtain the light electromagnetic shielding sealing material.
The electromagnetic shielding performance curves of the lightweight electromagnetic shielding sealing materials obtained in the numbers 1-5 to 1-9 are shown in FIG. 1.
TABLE 1 formulation and Properties for preparing lightweight electromagnetic shielding sealing material in example 1
Example 2
According to the formula shown in the table 2, taking the multi-walled carbon nanotube TNFN-8, adding 50g of ethanol, carrying out 100W ultrasonic dispersion for 5min, then rapidly adding the expanded microspheres Advancell EHM303, adding the aluminate coupling agent AD-50 according to 2% of the total mass of the microspheres and the multi-walled carbon nanotube, and mechanically stirring to uniformly disperse the mixture. And filtering the mixture by using a funnel, taking the solid, and transferring the solid to a blast oven to be dried at the temperature of 50 ℃ to obtain the microsphere-carbon nanotube composite powder.
And then adding a certain amount of microsphere-carbon nanotube composite powder into a mold cavity with the diameter of 30mm and the thickness of 15mm, keeping the temperature at 220 ℃ and the pressure at 5MPa for 15min, stopping heating, removing the pressure after the temperature is reduced to the room temperature, and opening the mold to obtain the light electromagnetic shielding sealing material.
TABLE 2 formulation and Properties of light electromagnetic shielding sealing material in example 2 (10.5975)
Example 3
Taking carbon nanofibers and expanded microspheres Advancell EM 501, wherein the weight ratio of the expanded microspheres to the carbon nanofibers is 4:1, adding the mixture into a mechanical stirring mixer, and adding titanate coupling agent YB-201 according to 1.5% of the total mass of the microspheres and the nanofibers to uniformly disperse the mixture to obtain microsphere-carbon nanofiber composite powder.
And then adding 6g of microsphere-carbon nanofiber composite powder into a mold cavity with the diameter of 30mm and the thickness of 15mm, keeping the temperature at 250 ℃ and the pressure at 10MPa for 5min, stopping heating, removing the pressure after the temperature is reduced to the room temperature, and opening the mold to obtain the light electromagnetic shielding sealing material.
The performance test shows that the density of the material is 0.566g/cm3The resistivity is 9.0 omega cm, the electromagnetic shielding performance is 65dB, and the compression strength is 1.5 MPa.
Example 4
Taking conductive carbon black and polymer expanded microspheres 051DU40, wherein the weight ratio of the expanded microspheres to the carbon black is 8:1, adding 30g of ethanol, adding a borate coupling agent PDR-180 according to 1% of the total mass of the microspheres and the carbon black, mechanically stirring to uniformly disperse the mixture, and airing at room temperature to obtain the microsphere-conductive carbon black composite powder.
And then adding 8.5g of microsphere-carbon black composite powder into a mold cavity with the diameter of 30mm and the thickness of 15mm, keeping the temperature at 180 ℃ and the pressure of 5-10 MPa for 25min, stopping heating, removing the pressure after the temperature is reduced to the room temperature, and opening the mold to obtain the cylindrical sample.
The performance test shows that the density of the material is 0.802g/cm3The resistivity is 32.5 omega cm, the electromagnetic shielding performance is 58dB, and the compression strength is 2.4 MPa.
In conclusion, the light electromagnetic shielding sealing material has the advantages of small density, excellent electric conduction and electromagnetic shielding performance and the like, is very suitable for being used as an electric conduction material and/or an electromagnetic shielding material, and has the advantages of simple preparation method, low energy consumption, high production efficiency and very good industrial prospect.
Claims (11)
1. A lightweight electromagnetic shielding sealing material characterized by: the preparation is prepared from the following raw materials: polymer expanded microspheres, carbon materials and coupling agents;
wherein the mass ratio of the polymer expanded microspheres to the carbon material is (8-2): 1, the mass of the coupling agent is 1-2% of the total mass of the polymer expanded microspheres and the carbon material;
the polymer expanded microsphere is selected from Akzo Nobel EXPANCELTM031DU40，AkzoNobel EXPANCEL TM051DU40, Advancell EHM303, Advancell EM 501;
the carbon material is selected from one or more of graphene, carbon nano tubes, conductive carbon black and carbon nano fibers;
the coupling agent is selected from: silane coupling agent, titanate coupling agent, aluminate coupling agent and borate coupling agent.
2. The lightweight electromagnetic shielding sealing material according to claim 1, wherein: the mass of the coupling agent is 2% of the total mass of the polymer expanded microspheres and the carbon material.
3. The lightweight electromagnetic shielding sealing material according to claim 1 or 2, characterized in that: the mass ratio of the polymer expanded microspheres to the carbon material is 2: 1.
4. the lightweight electromagnetic shielding sealing material according to claim 1 or 2, characterized in that: the polymer expanded microsphere is a hollow sphere which takes a thermoplastic polymer as a shell and a volatile organic compound as a core.
5. The lightweight electromagnetic shielding sealing material according to claim 1 or 2, characterized in that: the graphene is mechanically stripped graphene, and the carbon nano tube is a multi-wall carbon nano tube.
6. The lightweight electromagnetic shielding sealing material according to claim 1 or 2, characterized in that: it is composed of a hollow polymer spherical shell and a carbon material sandwiched between the spherical shells.
7. A method for preparing the light electromagnetic shielding sealing material of any one of claims 1 to 6, which is characterized by comprising the following steps: the method comprises the following steps:
i. taking raw materials, and uniformly dispersing to obtain intermediate powder;
and ii, adding the intermediate powder obtained in the step i into a mold cavity, and obtaining the light electromagnetic shielding sealing material under the conditions of temperature rise and pressure.
8. The method of claim 7, wherein: in step i, the uniform dispersion mode is as follows: taking raw materials, adding a solvent, mechanically stirring or ultrasonically dispersing, then filtering, and taking a solid; or, taking the raw materials, and mechanically stirring;
the solvent is selected from alcohol solvents or alcohol aqueous solutions.
9. The production method according to claim 7 or 8, characterized in that: in step ii, the temperature rise and pressure rise conditions are as follows: the temperature is 140-300 ℃, the pressure is the lowest pressure of 15MPa for keeping the mold cavity in a closed state, and the holding time is 3-60 min.
10. The method of claim 9, wherein: in step ii, the temperature rise and pressure rise conditions are as follows: the temperature is 160-250 ℃, the pressure is 2-10 MPa, and the holding time is 5-30 min.
11. Use of the lightweight electromagnetic shielding sealing material according to any one of claims 1 to 6 as a conductive material and/or an electromagnetic shielding material.
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| CN111607121A (en) * | 2020-06-02 | 2020-09-01 | 聊城大学 | Method for preparing electromagnetic shielding material based on expandable polymer microspheres |
| CN111876039B (en) * | 2020-06-30 | 2021-07-20 | 中国人民解放军军事科学院国防工程研究院工程防护研究所 | Self-layering radioactive pollution control and removal material, preparation method and application |
| CN115340744B (en) * | 2021-05-12 | 2023-06-20 | 中国科学院理化技术研究所 | Electromagnetic shielding composite material based on heterogeneous hollow microsphere layered enrichment and preparation method and application thereof |
| CN117447784A (en) * | 2023-11-08 | 2024-01-26 | 苏州市星辰新材料集团有限公司 | Permanent antistatic plastic packaging material and preparation method thereof |
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