CN110172260A - A kind of lightweight electromagnetic shielding sealing material and its preparation method and application - Google Patents
A kind of lightweight electromagnetic shielding sealing material and its preparation method and application Download PDFInfo
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- CN110172260A CN110172260A CN201910551361.8A CN201910551361A CN110172260A CN 110172260 A CN110172260 A CN 110172260A CN 201910551361 A CN201910551361 A CN 201910551361A CN 110172260 A CN110172260 A CN 110172260A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/041—Carbon nanotubes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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Abstract
The present invention provides a kind of lightweights to be electromagnetically shielded sealing material, it is prepared by following raw materials: polymer expandable microspheres, carbon material；Wherein, the mass ratio of polymer expandable microspheres and carbon material is (64~2): 1.Further, the raw material further includes coupling agent, and the quality of coupling agent is the 1%~2% of polymer expandable microspheres and carbon material gross mass, preferably 2%.Lightweight of the invention is electromagnetically shielded sealing material, and it is a variety of to have the advantages that density is small, conductive and electromagnetic shielding performance is excellent etc., is highly suitable as conductive material and electromagnetic shielding material.Moreover, the preparation method of lightweight electromagnetic shielding sealing material of the invention is easy, low energy consumption, high production efficiency, has very good industrialization prospect.
Description
Technical field
The invention belongs to macromolecule electromagnetic shielding material fields, and in particular to a kind of lightweight electromagnetic shielding sealing material and its
Preparation method and application.
Background technique
The appearance of electromagnetic wave has greatly facilitated social progress, and the development of hyundai electronics information technology and electromagnetic wave are close
It is inseparable.However, electronic equipment is widely used, a large amount of electromagnetic exposure and pollution are also resulted in, not only interferes electronics member device
The normal operation of part induces equipment fault, and meeting environmental pollution, endangers people's health, more seriously can also lead
Cause information leakage.
The reason of causing electronic equipment to generate electromagnetic exposure, is, between each element seam of constitution equipment, shell upper switch
Gap etc. does not obtain good shield gasket.It is then desired to explore and develop the figurate shielding material of tool to meet not
With the sealing demand in situation.
As the material for being able to satisfy shield gasket, it should have compressibility, conduction or magnetic conductivity, electromagnetic shielding or absorption
Etc. characteristics.It is commonly used for various field of sealing technology, this composite material Chang Xuan containing conductive or magnetic fillers rubber composite material
It is matrix with polyurethane, natural rubber, butyl rubber, ethylene propylene diene rubber elastomeric material, adds carbon nanotube, graphite
The fillers such as alkene, carbon fiber, metallized fibre, as made from specific processing method.In order to obtain required electromagnetic wave shielding
Can, the content of the filler in this kind of electromagnetic sealing material is higher, thus preparation cost is also higher.In order to when reducing cost
Excellent effectiveness is obtained, has research to attempt after preparing electromagnetic shield rubber composite material, then carry out foaming operation
(ACS Applied Materials&Interfaces, 2011,3:918-924；Nano letters, 2005,11:2131-
2134), conductive electromagnetic shielding performance is further increased, but to promote effect be not too ideal.Also research attempts soft
One layer of metal nanometer thin film (Chinese invention patent ZL201410414514.1, US are plated on the skeleton of matter open celled foam
6309742B1), splendid shield effectiveness can be both obtained under lower tenor in this way, also there is compressibility.But this
The chemical plating or electroplating technology that method is used, preparation process can generate a large amount of heavy metal pollution, and the metal on foam framework
There is also it is not corrosion-resistant the disadvantages of.The study found that forming continuous conductive network in composite inner helps to improve material
Electromagnetic shielding performance.Researcher develops isolation structure composite material, i.e., forms continuous filler in composite inner
Enrichment phase and resin matrix phase.For example, DX Yan et al. (Advanced Functional Materials, 2015,25:559-
566) by graphene-supported in polystyrene resin microsphere surface, then high-pressure, prepares under lower graphene dosage
The electromagnetic shielding composite material with isolation structure is gone out.But this method needs high pressure, can just make resin-bonding one
The mechanical strength for the material for rising, and obtaining is lower, is not suitable for industrialized production and application.
Summary of the invention
The splendid sealing material of electromagnetic performance is prepared in order to obtain a kind of simple method, present inventor passes through big
Quantifier elimination practice has unexpectedly obtained a kind of lightweight electromagnetic shielding sealing material, has achieved those skilled in the art and expect not
The technical effect arrived.
The purpose of the present invention is to provide a kind of lightweights to be electromagnetically shielded sealing material, it is characterised in that: it is by following originals
What material was prepared:
Polymer expandable microspheres, carbon material；
Wherein, the mass ratio of polymer expandable microspheres and carbon material is (64~2): 1.
Further, the raw material further includes coupling agent, and the quality of coupling agent is that polymer expandable microspheres and carbon material are total
The 1%~2% of quality, preferably 2%.
Further, the mass ratio of the polymer expandable microspheres and carbon material is (16~2): 1, preferably 2:1.
Further, the polymer expandable microspheres are one kind using thermoplastic polymer as shell, and volatile organic matter is core
Hollow sphere；
Preferably, the polymer expandable microspheres are selected from AkzoNobel EXPANCELTM031DU40, AkzoNobel
EXPANCELTMOne of 051DU40, Advancell EHM303, Advancell EM 501 or a variety of.
Further, the carbon material be selected from one of graphene, carbon nanotube, conductive black, carbon nano-fiber or
It is a variety of, it is preferable that the graphene is mechanical stripping graphene, and carbon nanotube is multi-walled carbon nanotube.
Further, the coupling agent is selected from: silane coupling agent, titanate coupling agent, aluminate coupling agent, borate are even
Join one of agent or a variety of.
Further, the lightweight electromagnetic shielding sealing material is by hollow polymer spherical shell and the carbon being clipped among spherical shell
Material is constituted.
The present invention also provides a kind of methods for preparing above-mentioned lightweight electromagnetic shielding sealing material, comprising the following steps:
I. raw material is taken, it is evenly dispersed, obtain intermediate powder；
Ii. the intermediate powder for taking step i to obtain is added in mold cavity, under heating, pressurized conditions, obtains lightweight electricity
Magnetic screen sealing material.
Further, in step i, the evenly dispersed mode are as follows: take raw material, solvent, mechanical stirring or ultrasound is added
Dispersion, then filters, takes solid；Or, raw material is taken, mechanical stirring；
The solvent is selected from alcohols solvent or alcohol solution；
And/or in step ii, the heating, pressurized conditions are as follows: temperature is 140 DEG C~300 DEG C, and pressure is to make mould type
Minimum pressure~15MPa that chamber is kept closed, retention time are 3~60min；Preferably, temperature is 160 DEG C~250 DEG C,
Pressure is 2~10MPa, and the retention time is 5~30min.
The present invention also provides above-mentioned lightweight electromagnetic shielding sealing materials as conductive material and/or electromagnetic shielding material
Using.
In the present invention, lightweight is electromagnetically shielded the forming process of sealing material are as follows: at high temperature, polymer expandable microspheres spherical shell
Softening, internal low-boiling-point organic compound volatilization, makes microsphere expansion, carbon material is extruded among polymer spherical shell.Further, since carbon
Material is random dispersion, does not have the place of carbon material between ball and ball, polymeric shells mutual extrusion and bond together, make
Obtaining resulting materials has certain interfacial adhesion strength.
The invention has the following advantages:
(1) Inventive polymers are expanded to matrix, and under the driving of expansive force, carbon material is clipped in the polymer drops to swell
Between shell, preparation method is extremely simple, it is easy to accomplish, it is very suitable to scale application；
(2) the lightweight electromagnetic shielding sealing material obtained by the present invention is under less carbon material dosage, so that it may obtain
Excellent shield effectiveness, and resulting materials overall cost is cheap；
(3) the obtained electromagnetic shielding sealing material of the present invention is light, the minimum reachable 0.3g/cm3 of density；
(4) the obtained electromagnetic shielding sealing material electric conductivity of the present invention is fabulous, the minimum reachable 0.01 Ω cm of resistivity；
(5) the obtained electromagnetic shielding sealing material electromagnetic shielding performance of the present invention is splendid, within the scope of 0.05~20GHz
Electromagnetic shielding performance reaches as high as 120dB.
Lightweight of the invention is electromagnetically shielded sealing material, has small density, electric conductivity and electromagnetic shielding performance excellent, and property
A variety of advantages such as energy is adjustable are highly suitable as the application of conductive material and/or electromagnetic shielding material, and preparation method letter
Just, environmental protection, low energy consumption, high production efficiency, have very good industrialization prospect.
Obviously, above content according to the present invention is not being departed from according to the ordinary technical knowledge and customary means of this field
Under the premise of the above-mentioned basic fundamental thought of the present invention, the modification, replacement or change of other diversified forms can also be made.
The specific embodiment of form by the following examples remakes further specifically above content of the invention
It is bright.But the range that this should not be interpreted as to the above-mentioned theme of the present invention is only limitted to example below.It is all to be based on above content of the present invention
The technology realized all belongs to the scope of the present invention.
Detailed description of the invention
Fig. 1 is the electromagnetic shielding that number is the electromagnetic shielding sealing material of lightweight obtained by 1-5 to 1-9 in the embodiment of the present invention 1
Performance curve.
Specific embodiment
Raw materials used in the embodiment of the present invention, equipment can be obtained by purchase commercial product.
One, primary raw material
1, polymer expandable microspheres: AkzoNobel EXPANCELTM031DU40,051DU40；Advancell
EHM303, EM 501.
2, carbon material: mechanical stripping graphene (HE01, Chengdu olefinic carbon science and technology)；Multi-walled carbon nanotube (TNFN-8, the Chinese Academy of Sciences
Chengdu organic chemistry research institute)；Conductive black (Anyang moral Long Huagong)；Carbon nano-fiber (Beijing Deco island gold science and technology).
3, coupling agent: Silane coupling agent KH550, titanate coupling agent YB-201, aluminate coupling agent AD-50, borate
Coupling agent LD-100P.
Two, performance test
1, the resistance of gained circular disc test specimen is tested using multimeter, and calculates electricalresistivityρ according to the following formula:
R is resistance；R is radius, and L is thickness.
2, according to coaxial method principle, circular disc test specimen is measured using KEYSIGHT PNA-X N5247A vector network analyzer
Electromagnet shield effect, scanning band be 0.05~20GHz, specimen finish 11mm, with a thickness of 2mm.
3, the apparent density of weight method test sample；
4, the compression performance of cylinder sample (30 × 15mm of φ) is tested using 4302 type universal material experimental machine of INSTRON,
Sensor is 30KN, test speed 2mm/min, with strain be 10% when compressive strength measure the mechanical property of sample.
Embodiment 1
It is formulated by table 1, takes polymer expandable microspheres 031DU40, mechanical stripping graphene, addition 20g concentration is 75vol%
Ethanol/water mixture, coupling agent KH550 is added by the 2% of the gross mass of microballoon and graphene, mechanical stirring makes mixture point
It dissipates uniform.Then it is filtered with funnel, takes solid, transferred in convection oven and dried at 60 DEG C, it is multiple to obtain microballoon-graphene
Close powder.
Taking a certain amount of microballoon-graphene composite powder that diameter is added is 30mm, with a thickness of in the mold cavity of 15mm, in temperature
Under conditions of degree is 160 DEG C, pressure is 2MPa, stops heating after keeping the temperature 30min, is cooled to room temperature at a temperature of, removes pressure,
Die sinking is electromagnetically shielded sealing material to get to the lightweight.
The electromagnetic shielding performance curve of the electromagnetic shielding sealing material of lightweight obtained by number 1-5 to 1-9 is as shown in Figure 1.
The preparation formula and performance of lightweight electromagnetic shielding sealing material in 1 embodiment 1 of table
Embodiment 2
It is formulated by table 2, takes multi-walled carbon nanotube TNFN-8, be added 50g ethyl alcohol, 100W ultrasonic disperse 5min, then rapidly
Expandable microspheres Advancell EHM303 is added, aluminate coupling agent is added by the 2% of microballoon and multi-walled carbon nanotube gross mass
AD-50, mechanical stirring make mixture be uniformly dispersed.Then it is filtered with funnel, takes solid, transferred in convection oven in 50 DEG C
Lower drying obtains microballoon-carbon nano-tube composite powder end.
Then taking a certain amount of microballoon-carbon nano-tube composite powder end that diameter is added is 30mm, with a thickness of the mold cavity of 15mm
In, under the conditions of temperature is 220 DEG C, pressure is 5MPa, stops heating after keeping the temperature 15min, be cooled to room temperature, remove at a temperature of
Pressure, die sinking are electromagnetically shielded sealing material to get to the lightweight.
The preparation formula and performance (10.5975) of lightweight electromagnetic shielding sealing material in 2 embodiment 2 of table
Embodiment 3
Carbon nano-fiber, expandable microspheres Advancell EM 501 are taken, expandable microspheres and carbon nano-fiber weight ratio are 4:
1, it is added in mechanical stirring mixer, titanate coupling agent YB-201 is added by the 1.5% of microballoon and nanofiber gross mass, makes
Mixture is uniformly dispersed, and obtains microballoon-carbon nano-fiber composite powder.
Then taking 6g microballoon-carbon nano-fiber composite powder that diameter is added is 30mm, with a thickness of in the mold cavity of 15mm,
Under the conditions of temperature is 250 DEG C, pressure is 10MPa, stops heating after keeping the temperature 5min, be cooled to room temperature at a temperature of, remove pressure
Power, die sinking are electromagnetically shielded sealing material to get to the lightweight.
Performance test shows that the density of material is 0.566g/cm3, resistivity is 9.0 Ω cm, electromagnetic shielding performance
65dB, compressive strength 1.5MPa.
Embodiment 4
Conductive black, polymer expandable microspheres 051DU40 are taken, expandable microspheres and carbon black weight ratio are 8:1, and 30g second is added
Alcohol, then boric acid ester coupler PDR-180 is added by the 1% of microballoon and carbon black gross mass, mechanical stirring makes mixture be uniformly dispersed,
It dries at room temperature, obtains microballoon-conductive black composite powder.
Then 8.5g microballoon-carbon black composite powder is taken, addition diameter is 30mm, with a thickness of in the mold cavity of 15mm,
Under the conditions of temperature is 180 DEG C, pressure is 5~10MPa, stops heating after keeping the temperature 25min, be cooled to room temperature, remove at a temperature of
Pressure is simultaneously opened to get cylindric sample is arrived.
Performance test shows that the density of material is 0.802g/cm3, resistivity is 32.5 Ω cm, electromagnetic shielding performance
58dB, compressive strength 2.4MPa.
In conclusion lightweight of the invention is electromagnetically shielded sealing material, have that density is small, conductive and electromagnetic shielding performance is excellent
A variety of advantages such as good, are highly suitable as the application of conductive material and/or electromagnetic shielding material, moreover, lightweight epoxy of the present invention
The preparation method of resin composite materials is easy, and low energy consumption, high production efficiency, has very good industrialization prospect.
Claims (10)
1. a kind of lightweight is electromagnetically shielded sealing material, it is characterised in that: it is prepared by following raw materials: polymer expansion
Microballoon, carbon material；
Wherein, the mass ratio of polymer expandable microspheres and carbon material is (64~2): 1.
2. lightweight according to claim 1 is electromagnetically shielded sealing material, it is characterised in that: the raw material further includes coupling
Agent, the quality of coupling agent are the 1%~2% of polymer expandable microspheres and carbon material gross mass, preferably 2%.
3. lightweight according to claim 1 or 2 is electromagnetically shielded sealing material, it is characterised in that: the polymer expansion is micro-
The mass ratio of ball and carbon material is (16~2): 1, preferably 2:1.
4. lightweight according to claim 1 or 2 is electromagnetically shielded sealing material, it is characterised in that: the polymer expansion is micro-
Ball is one kind using thermoplastic polymer as shell, and volatile organic matter is the hollow sphere of core；
Preferably, the polymer expandable microspheres are selected from AkzoNobel EXPANCELTM031DU40, AkzoNobel
EXPANCELTMOne of 051DU40, Advancell EHM303, Advancell EM 501 or a variety of.
5. lightweight according to claim 1 or 2 is electromagnetically shielded sealing material, it is characterised in that: the carbon material is selected from stone
One of black alkene, carbon nanotube, conductive black, carbon nano-fiber are a variety of, it is preferable that the graphene is mechanical stripping stone
Black alkene, carbon nanotube are multi-walled carbon nanotube.
6. lightweight according to claim 1 or 2 is electromagnetically shielded sealing material, it is characterised in that: the coupling agent is selected from: silicon
One of alkane coupling agent, titanate coupling agent, aluminate coupling agent, boric acid ester coupler are a variety of.
7. described in any item lightweights are electromagnetically shielded sealing material according to claim 1~6, it is characterised in that: it is by hollow
Polymer spherical shell and the carbon material being clipped among spherical shell are constituted.
8. a kind of method for preparing any one of claim 1~7 lightweight electromagnetic shielding sealing material, it is characterised in that: packet
Include following steps:
I. raw material is taken, it is evenly dispersed, obtain intermediate powder；
Ii. the intermediate powder for taking step i to obtain is added in mold cavity, under heating, pressurized conditions, obtains lightweight electromagnetic screen
Cover sealing material.
9. preparation method according to claim 8, it is characterised in that: in step i, the evenly dispersed mode are as follows: take
Raw material is added solvent, mechanical stirring or ultrasonic disperse, then filters, take solid；Or, raw material is taken, mechanical stirring；
The solvent is selected from alcohols solvent or alcohol solution；
And/or in step ii, the heating, pressurized conditions are as follows: temperature is 140 DEG C~300 DEG C, and pressure is to protect mold cavity
Minimum pressure~15MPa of closed state is held, the retention time is 3~60min；Preferably, temperature is 160 DEG C~250 DEG C, pressure
For 2~10MPa, the retention time is 5~30min.
10. any one of the claim 1~7 lightweight electromagnetic shielding sealing material is as conductive material and/or electromagnetic shielding material
The application of 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 |
| CN111876039A (en) * | 2020-06-30 | 2020-11-03 | 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 |
| CN115340744A (en) * | 2021-05-12 | 2022-11-15 | 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111876039A (en) * | 2020-06-30 | 2020-11-03 | 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 |
| CN115340744A (en) * | 2021-05-12 | 2022-11-15 | 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 |
| 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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