CN117165253A - High-low temperature resistant electromagnetic shielding adhesive and preparation method thereof - Google Patents
High-low temperature resistant electromagnetic shielding adhesive and preparation method thereof Download PDFInfo
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- CN117165253A CN117165253A CN202311179038.5A CN202311179038A CN117165253A CN 117165253 A CN117165253 A CN 117165253A CN 202311179038 A CN202311179038 A CN 202311179038A CN 117165253 A CN117165253 A CN 117165253A
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- 238000000034 method Methods 0.000 claims abstract description 23
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- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention belongs to the technical field of electromagnetic shielding materials, and particularly relates to a high-low temperature resistant electromagnetic shielding adhesive and a preparation method thereof; the high-low temperature resistant electromagnetic shielding adhesive is prepared from an electromagnetic shielding adhesive A component and an electromagnetic shielding adhesive B component according to a ratio of 10:1, wherein the electromagnetic shielding adhesive A component consists of silicon rubber, epoxy resin, polyaniline, silver-coated copper powder, carbon nanotubes, conductive zinc oxide, gasoline, butyl titanate, KYC913 and organic tin; the electromagnetic shielding adhesive B consists of tetraethoxysilane, polyethylene polyamine and gasoline. The electromagnetic shielding glue does not contain precious metals such as gold and silver, so that the production cost is greatly reduced, and the process is simple and easy to control; the electromagnetic shielding adhesive has good high temperature resistance of 300 ℃, low temperature resistance of-45 ℃ and conductivity, can greatly improve the isolation degree and the phase sensitivity of an antenna when used on the antenna of an aerospace vehicle, and has higher electromagnetic shielding effect when used on a fragile cover of a transmitting box in a certain frequency band.
Description
Technical Field
The invention belongs to the technical field of electromagnetic shielding materials, and particularly relates to a high-low temperature resistant electromagnetic shielding adhesive and a preparation method thereof.
Background
The electromagnetic shielding adhesive is an adhesive with certain conductive performance after solidification or drying, and generally takes matrix resin and conductive filler, namely conductive particles, as main components, and the conductive particles are combined together through the bonding action of the matrix resin to form a conductive path so as to realize conductive connection of the adhered materials. The matrix resin of the electromagnetic shielding glue is an adhesive, so that the electromagnetic shielding glue can be bonded at a proper curing temperature, and meanwhile, the electromagnetic shielding glue can be made into slurry to realize high line resolution due to miniaturization and microminiaturization of electronic elements and rapid development of high density and high integration of printed circuit boards. And the electromagnetic shielding glue has simple process, is easy to operate and can improve the production efficiency, so the electromagnetic shielding glue is an ideal choice for replacing lead-tin welding and realizing conductive connection.
The electromagnetic shielding glue mainly comprises a resin matrix, conductive particles, a dispersing additive, an auxiliary agent and the like. The matrix mainly comprises epoxy resin, acrylic resin, polychlorinated ester and the like. Although the high conjugated polymer itself has conductivity, such as macromolecular pyridine structure, etc., and can conduct electricity through electrons or ions, the conductivity of the electromagnetic shielding glue can only reach the degree of a semiconductor at most, and the electromagnetic shielding glue can not have low resistance like metal, and is difficult to play a role of conducting connection. Electromagnetic shielding adhesives used in the current market are mostly filler type. The resin matrix of the filler type electromagnetic shielding glue can be a resin matrix of various glue types in principle, and commonly used thermosetting adhesives such as silicone rubber, epoxy resin, organic silicon resin, polyimide resin, phenolic resin, polyurethane, acrylic resin and other adhesive systems are generally used; the synthetic rubber commonly used in the electromagnetic shielding rubber is silicon rubber, natural rubber and top rubber. The adhesives form a molecular skeleton structure of the electromagnetic shielding adhesive after being cured, so that the mechanical property and the bonding property are ensured, and conductive filler particles form channels. Because the bond energy of the silicone rubber is large, the temperature range of the silicone rubber is very wide, the heat resistance temperature can reach 400 ℃ after the phenyl is introduced, and meanwhile, the raw silicone rubber molecular structure is spiral, and the flexibility is good, so that the silicone rubber has good low temperature resistance. The silicone rubber has high and low temperature resistance, ageing resistance, electrical property, hydrophobicity, air permeability, chemical stability, biocompatibility, compression permanent deformation resistance and radiation resistance, and the silicone rubber is used as a high and low temperature resistant conductive matrix to solve the high and low temperature resistance of the electromagnetic shielding rubber.
The conductive medium of the electromagnetic shielding glue can be made of conductive materials such as gold, silver, copper, aluminum, graphite, carbon black and the like, and the resistivity of the gold and the silver is low, so that the conductive medium is an ideal material for manufacturing the electromagnetic shielding glue, but the noble metals of the gold and the silver can increase the manufacturing cost of the electromagnetic shielding glue. Copper and aluminum are easy to oxidize in air, and the oxide is not conductive, so that the conductivity and the service life of the electromagnetic shielding glue are affected. The chemical properties of graphite and carbon black in air are stable, the influence of acid-base medium is small, the electric conductivity of graphite is hundreds of times higher than that of common nonmetallic ores, and the heat conductivity of graphite exceeds that of metallic materials such as steel, iron, lead and the like. The thermal conductivity decreases with increasing temperature and even at very high temperatures, graphite forms a thermal insulator. Graphite is capable of conducting electricity because each carbon atom in graphite forms only 3 covalent bonds with other carbon atoms, and each carbon atom still retains 1 free electron to transport charge, and research has begun into the use of graphite in electromagnetic shielding glue products. The patent document with publication number CN103409083B discloses a graphite carbon black electromagnetic shielding glue and a preparation method thereof, wherein high polymer resin is used as matrix resin, graphite and super-conductive carbon black are used as conductive filler, and curing agent, accelerator and solvent are used as auxiliary materials to prepare the electromagnetic shielding glue. Although the patent proves that the electromagnetic shielding glue prepared from the graphite can improve the temperature resistance of the electromagnetic shielding glue, the electromagnetic shielding glue has low resistivity and short temperature resistance time, and the highest temperature resistance is 80 ℃ and the lowest temperature resistance is-30 ℃, so that the electromagnetic shielding glue is not beneficial to the use on an aircraft antenna.
Another important component in electromagnetic shielding glue is solvent. Because the addition of the conductive filler is at least more than 50%, the viscosity of the resin matrix of the electromagnetic shielding adhesive is greatly increased, and the process performance of the adhesive is often affected. In order to reduce the viscosity and achieve good manufacturability and rheological properties, besides the low-viscosity resin, a solvent or a reactive diluent is generally required to be added, wherein the reactive diluent can be directly used as a resin matrix for reaction curing. Although the amount of the solvent or reactive diluent is not large, it plays an important role in the electromagnetic shielding paste, and affects not only the conductivity but also the mechanical properties of the cured product. The solvents (or diluents) used generally should have a relatively large molecular weight, be relatively slow to volatilize, and contain polar structures such as carbon-oxygen polar chains in the molecular structure. The addition amount of the solvent is controlled within a certain range so as not to influence the adhesive joint overall performance of the electromagnetic shielding adhesive.
Besides the resin matrix, the conductive filler and the diluent, other components of the electromagnetic shielding adhesive are the same as the adhesive, and the electromagnetic shielding adhesive also comprises a cross-linking agent, a coupling agent, a preservative, a toughening agent, a thixotropic agent and the like.
The original silicon rubber with a certain brand produced by a certain research institute is used for bonding by a company, the bonding strength, the high-temperature conductivity and the high-temperature resistivity of the adhesive are low after the adhesive is used, in addition, the defects in the construction process exist, the adhesive is not easy to detach and remove in the reverse operation process, the residual adhesive is not easy to clean, the damage to electronic devices is easy to cause, the price is high, and the production cost is high. The electromagnetic shielding glue in the current market is mainly conductive by adding gold, silver, copper, aluminum, zinc, iron, nickel powder and the like, but the addition of a large amount of heavy metals greatly increases the production cost and also can influence the health of human bodies and pollute the environment.
Disclosure of Invention
The invention aims to solve the problems, and provides the high-low temperature resistant electromagnetic shielding adhesive and the preparation method thereof, wherein the production process is simple to operate, easy to control, low in cost and environment-friendly, so that the problems that the adhesive strength and electromagnetic shielding efficiency of the conventional electromagnetic shielding adhesive are low, residual adhesive is difficult to clean, and electronic devices are easy to damage are solved.
The method is realized by the following technical scheme:
a high-low temperature resistant electromagnetic shielding adhesive and a preparation method thereof comprise the following steps:
the high-low temperature resistant electromagnetic shielding adhesive consists of the following components in percentage by mass: the component A of the electromagnetic shielding adhesive and the component B of the electromagnetic shielding adhesive are 10:1;
the electromagnetic shielding agent A component consists of the following raw materials in parts by weight:
80-100 parts of silicon rubber, 0-20 parts of epoxy resin, 0-15 parts of polyaniline, 80-100 parts of silver-coated copper powder, 0-1 part of carbon nano tube, 45-55 parts of conductive graphite, 25-35 parts of acetylene black, 15-35 parts of zinc oxide, 10-50 parts of gasoline, 0.2-0.5 part of butyl titanate and 0.2-0.5 part of KYC 913.
The electromagnetic shielding adhesive B component consists of the following raw materials in parts by weight:
4 to 8 parts of tetraethoxysilane, 10 to 20 parts of polyethylene polyamine, 0.1 to 0.3 part of organic tin and 1.2 to 3.7 parts of gasoline.
Further, the methyl diphenyl sulfide silicone rubber is HTY-PR310H methyl diphenyl sulfide silicone rubber as an adhesive base material.
The epoxy resin mark is E51 and is used as an adhesive matrix material.
The specification of the silver-coated copper powder is industrial grade flake, silver content is 10%, particle size is 1000 meshes, and the silver-coated copper powder is used as filler.
The specification of the carbon nano-tube is that the multi-wall and nano-scale carbon nano-tube is used as a filler.
The polyaniline is in a conductive state, and the polyaniline is used as a filler.
The zinc oxide is conductive zinc oxide with a tetrapod-like structure as a filler.
The graphite is conductive graphite with 1000-2500 meshes and is used as a filler.
The carbon black is acetylene carbon black and is used as a filler.
The gasoline is 120# aviation gasoline as a solvent.
The butyl titanate is CP butyl titanate as a coupling agent.
The KYC913 acts as a nanomaterial dispersant.
The butyl tin dilaurate is AR butyl tin dilaurate as a catalyst.
The ethyl orthosilicate is CP ethyl orthosilicate as a cross-linking agent.
The preparation method of the high-low temperature resistant electromagnetic shielding glue comprises the following steps:
1) The preparation method of the electromagnetic shielding adhesive A comprises the following steps:
a) Weighing, stirring and mixing: weighing methyl diphenyl silicon sulfide rubber, epoxy resin, silver-coated copper powder, conductive zinc oxide, carbon nanotubes, polyaniline, butyl titanate and gasoline according to a formula ratio, placing the materials into a pulling cylinder of a dispersing machine, starting the dispersing machine, and stirring and dispersing for 30min at a rotating speed of 600 revolutions per minute;
b) Grinding: adjusting the distance between the front grinding roller and the rear grinding roller of the three-roller grinding machine, opening condensed water, starting the grinding machine, and enabling the rotating speed of the grinding machine to be 1000 revolutions per minute; adding the electromagnetic shielding adhesive after stirring in the step a) to the back roller of the regulated three-roller grinder for grinding, adding the electromagnetic shielding adhesive at the front roller discharge port of the three-roller grinder to the back roller for grinding after finishing grinding, repeatedly grinding for 4 times, and packaging after finishing grinding to obtain an electromagnetic shielding adhesive A component;
c) Cleaning three rollers of the three-roller grinder by using gasoline, and closing condensed water and the three-roller grinder;
2) The preparation method of the electromagnetic shielding adhesive B comprises the following steps:
a) Weighing: weighing tetraethoxysilane, polyethylene polyamine, organic tin dilaurate and gasoline according to the formula ratio;
b) Stirring and dispersing: adding tetraethoxysilane, polyethylene polyamine, organic tin dilaurate and gasoline into a pulling cylinder of a dispersing machine, starting the dispersing machine, absorbing, stirring and dispersing for 20min at the rotating speed of 600 revolutions per minute, and packaging after stirring and dispersing are finished to obtain a component B;
3) During construction, the component A and the component B of the electromagnetic shielding adhesive are prepared according to a ratio of 10:1, and are cured for 96 hours at room temperature after construction.
In summary, the beneficial effects of the invention are as follows: the high-low temperature resistant electromagnetic shielding adhesive is used at the joint of the surface of the aircraft, the mounting gap of the antenna and the surface of the fragile cover of the transmitting cylinder, so that the conductive continuity of the surface of the aircraft is realized, the electronic devices inside the aircraft are prevented from being interfered by external electromagnetic waves, and the phase characteristics among receiving and transmitting antennas of the aircraft equipment are ensured, so that the electromagnetic shielding requirement of the aircraft is met. The production process and the construction process are simple; the material is solidified at room temperature, has low energy consumption, avoids damaging a base material, and can be applied to materials sensitive to temperature or materials which cannot be welded; good wettability with most of the adhered materials; the electromagnetic shielding, shock absorption, sealing and bonding performances are good; the temperature application range is wide (-45 ℃ to 300 ℃); the antenna isolation and phase sensitivity are greatly improved when the antenna is installed on an aircraft; the electromagnetic shielding glue does not contain heavy metals such as gold, silver and the like, and greatly reduces the manufacturing cost.
The electromagnetic shielding adhesive used in the invention has a wider use temperature range, the methyl diphenyl silicon sulfide rubber can keep elasticity at low temperature, has good radiation resistance, ablation resistance and self-extinguishing property at room temperature, and has heat resistance at high temperature. The methyl diphenyl silicon sulfide rubber and the epoxy resin are matched with silver-coated copper powder, conductive polyaniline, carbon nano tubes and conductive zinc oxide powder for use, so that the conductivity and the stretching rate of the composite material are enhanced.
When the component A of the electromagnetic shielding adhesive is prepared, the formula is repeatedly ground for 4 times by a three-roller grinder at the rotating speed of 1000 revolutions per minute, so that the electromagnetic shielding adhesive is finer, the compatibility between raw materials is improved, and the fluidity and the elasticity are improved.
The invention uses butyl phthalate as a coupling agent, the reactivity of the hydrolyzable groups of the butyl phthalate and the fixability of the carbon groups on the surface of the organic material, wherein a part of functional groups react with organic molecules to form a bridge between the resin and the interface, the adhesive force of the paint and the adhesive is increased, the use amount is small, and the compatibility and the dispersibility of raw materials such as methyl diphenyl silicon sulfide rubber, silver coated copper powder, carbon nano tubes, conductive zinc oxide powder and the like are improved.
According to the invention, butyl tin dilaurate is used as a catalyst, and ethyl orthosilicate is matched, so that the curing condition of the system is reduced, the curing rate is accelerated, and the curing can be performed at room temperature. And the butyl tin dilaurate has excellent lubricating property, transparency, weather resistance and other properties, and the quality of the product is further improved.
The invention prepares the high and low temperature resistant electromagnetic shielding collagen material with the dosage ratio according to the nature of raw materials and the product requirement, and takes methyl diphenyl silicon sulfide rubber as an electromagnetic shielding rubber substrate to add filler, solvent, coupling agent, drier and cross-linking agent according to the required dosage. When the addition amount of the conductive powder is too small, the silver-coated copper powder, the carbon nano tube and the conductive zinc oxide powder cannot be connected in a chain shape, a conductive loop cannot be formed, so that the non-conduction or the very small conductivity is caused, the electromagnetic shielding performance cannot reach the requirement, the viscosity of the glue solution with too large dosage becomes large, the dispersion and the use are not facilitated, the adhesive force of the electromagnetic shielding glue is reduced, and the heat resistance is also reduced. The organic solvent gasoline is used for adjusting the viscosity of the electromagnetic shielding colloid system, reducing the surface tension, leading the whole system to be uniform and fine, reducing the content of the electromagnetic shielding colloid system due to the excessive use level, reducing the viscosity, causing uneven dispersion of the system due to the excessive use level, and not meeting the requirements. The component A of the electromagnetic shielding adhesive is mainly used for adjusting the viscosity of an electromagnetic shielding adhesive system by using gasoline, and the component B of the electromagnetic shielding adhesive is mainly used for dissolving and dispersing by using gasoline.
The conductive particles are contacted with each other to form a conductive path, so that the electromagnetic shielding glue has conductivity, and the stable contact between the particles in the glue layer is caused by curing or drying the electromagnetic shielding glue. Before curing or drying, the conductive particles are separated in the adhesive and are not in continuous contact with each other, so that the electromagnetic shielding adhesive is in an insulating state. After the electromagnetic shielding glue is solidified or dried, the volume of the adhesive is contracted due to the volatilization of the solvent and the solidification of the adhesive, so that the conductive particles are in a stable continuous state, and the conductivity is shown.
The high-low temperature resistant electromagnetic shielding adhesive is prepared from an electromagnetic shielding adhesive A component and an electromagnetic shielding adhesive B component in a ratio of 10:1, wherein the electromagnetic shielding adhesive B component is used as an auxiliary adhesive A component for preparation, and the high-low temperature resistant electromagnetic shielding adhesive has the characteristics of excellent elasticity, bonding strength, heat resistance and wear resistance. The tetraethoxysilane in the component B of the electromagnetic shielding adhesive is used as a cross-linking agent of silicon rubber, the polyethylene polyamine is used as an epoxy resin curing agent, the organic tin dilaurate is used as a catalyst, and the cross-linking curing agent in the component B of the gasoline is diluted, so that the chemical active functional groups in the component A of the electromagnetic shielding adhesive are mutually connected to form a network structure, and the elasticity, the strength, the wear resistance and the heat resistance of the electromagnetic shielding adhesive are improved. The component B of the electric adhesive assists the electric adhesive to carry out curing reaction by the component A of the electromagnetic shielding adhesive, the elasticity of the electromagnetic shielding adhesive is reduced, the tensile strength is reduced, the elongation at break is reduced, the electromagnetic shielding adhesive is hardened, the product requirement of the electromagnetic shielding adhesive is not met, and when the concentration of the cross-linking agent is too high, the cross-linking agent can act with a conductive filler network, so that the conductive performance of the electromagnetic shielding adhesive is reduced. The electromagnetic shielding adhesive is high due to the fact that the amount is too low, so that the electromagnetic shielding adhesive is not easy to detach and the residual adhesive is not easy to clean. Therefore, the use of reasonable raw material dosage ranges is also a key technology for manufacturing products meeting the requirements of the products.
Detailed Description
The following detailed description of the invention is provided in further detail, but the invention is not limited to these embodiments, any modifications or substitutions in the basic spirit of the present examples, which still fall within the scope of the invention as claimed.
Example 1
1.1 high and low temperature resistant electromagnetic shielding adhesive is composed of the following formula ratio: the electromagnetic shielding adhesive A component and the electromagnetic shielding adhesive B component are 100:7.
1.2 preparation method of high and low temperature resistant electromagnetic shielding adhesive comprises the following steps of
1) The preparation method of the electromagnetic shielding adhesive A comprises the following steps:
a) Weighing, stirring and mixing: weighing 100kg of methyl diphenyl silicon sulfide rubber, 55kg of conductive graphite powder, 35kg of acetylene black, 0.5kg of butyl titanate and 150kg of gasoline according to the formula ratio, placing the materials into a pulling cylinder of a dispersing machine, starting the dispersing machine, and stirring and dispersing for 30min at the rotating speed of 600 revolutions per minute;
b) Grinding: adjusting the distance between the front grinding roller and the rear grinding roller of the three-roller grinding machine, opening condensed water, starting the grinding machine, and enabling the rotating speed of the grinding machine to be 1000 revolutions per minute; adding the electromagnetic shielding adhesive after stirring in the step a) to the back roller of the regulated three-roller grinder for grinding, adding the electromagnetic shielding adhesive at the front roller discharge port of the three-roller grinder to the back roller for grinding after finishing grinding, repeatedly grinding for 4 times, and packaging after grinding to obtain an electromagnetic shielding adhesive A component;
c) Cleaning three rollers of the three-roller grinder by using gasoline, and closing condensed water and the three-roller grinder;
2) The preparation method of the electromagnetic shielding adhesive B comprises the following steps:
a) Weighing: 8kg of ethyl orthosilicate, 0.3kg of butyl tin dilaurate and 3.7kg of gasoline are weighed according to the formula ratio;
b) Stirring and dispersing: after weighing, adding tetraethoxysilane, butyl tin dilaurate and gasoline into a pulling cylinder of a dispersing machine, starting the dispersing machine, absorbing, stirring and dispersing for 20min at the rotating speed of 600 revolutions per minute, and packaging after stirring and dispersing are finished to obtain a component B;
3) The electromagnetic shielding adhesive is prepared from an electromagnetic shielding adhesive A component and an electromagnetic shielding adhesive B component in a ratio of 100:7 when the electromagnetic shielding adhesive is to be constructed, and is cured for 96 hours at room temperature to be completely cured, so that the electromagnetic shielding adhesive is prepared.
The resistivity of the electromagnetic shielding glue prepared in example 1 is 4.6X10 -3 Omega.m, shielding effectiveness-7 dB (K wave), and bonding strength on polyurethane plastic of 0.6Mpa.
Example 2
2.1 high and low temperature resistant electromagnetic shielding adhesive is composed of the following formula ratio: the component A of the electromagnetic shielding adhesive and the component B of the electromagnetic shielding adhesive are 10:1;
2.2, the preparation method of the high-low temperature resistant electromagnetic shielding glue comprises the following steps:
1) The preparation method of the electromagnetic shielding adhesive A comprises the following steps:
a) Weighing, stirring and mixing: weighing 10kg of gasoline according to the formula ratio, adding 0.5kg of butyl titanate and 0.2kg of KYC913 into a dispersing agent drawing cylinder, absorbing, stirring and dispersing for 20min at the rotating speed of 600 rpm, and then adding 0.5kg of carbon nano tube and continuing stirring for 30min.
b) Adding 80kg of silicon rubber and 5kg of epoxy resin into a), continuously stirring for 30min, then sequentially adding 80kg of silver-coated copper powder, 25kg of conductive zinc oxide (common conductive type) and 15kg of polyaniline, and continuously stirring for 60min;
c) Grinding: adjusting the distance between the front grinding roller and the rear grinding roller of the three-roller grinding machine, opening condensed water, starting the grinding machine, and enabling the rotating speed of the grinding machine to be 1000 revolutions per minute; adding the electromagnetic shielding adhesive after stirring in the step a) to the back roller of the regulated three-roller grinder for grinding, adding the electromagnetic shielding adhesive at the front roller discharge port of the three-roller grinder to the back roller for grinding after finishing grinding, repeatedly grinding for 4 times, and packaging after grinding to obtain an electromagnetic shielding adhesive A component;
c) Cleaning three rollers of the three-roller grinder by using gasoline, and closing condensed water and the three-roller grinder;
2) The preparation method of the electromagnetic shielding adhesive B comprises the following steps:
a) Weighing: weighing 8kg of ethyl orthosilicate, 1kg of polyethylene polyamine, 0.3kg of organic tin dilaurate and 3.7kg of gasoline according to the formula ratio;
b) Stirring and dispersing: after weighing, adding tetraethoxysilane and 120# gasoline into a pull cylinder in a dispersing machine, starting the dispersing machine, absorbing, stirring and dispersing for 20min at the rotating speed of 600 revolutions per minute, and packaging after stirring and dispersing are finished to obtain a component B;
3) The electromagnetic shielding adhesive is prepared from an electromagnetic shielding adhesive A component and an electromagnetic shielding adhesive B component in a ratio of 10:1 when the electromagnetic shielding adhesive is to be constructed, and is cured for 96 hours at room temperature after an active period of 3 hours to be completely cured, so that the electromagnetic shielding adhesive is prepared.
The resistivity of the electromagnetic shielding adhesive prepared in example 2 is 2 multiplied by 10 -5 Omega.m, shielding effectiveness-14 dB (K wave), and bonding strength on polyurethane easy plastic of 1.3Mpa.
Example 3
3.1 high and low temperature resistant electromagnetic shielding adhesive is composed of the following formula ratio: the component A of the electromagnetic shielding adhesive and the component B of the electromagnetic shielding adhesive are 10:1;
3.2, the preparation method of the high-low temperature resistant electromagnetic shielding adhesive comprises the following steps:
1) The preparation method of the electromagnetic shielding adhesive A comprises the following steps:
a) Weighing, stirring and mixing: weighing 10kg of gasoline according to the formula ratio, adding 0.5kg of butyl titanate and 0.2kg of KYC913 into a dispersing agent drawing cylinder, absorbing, stirring and dispersing for 20min at the rotating speed of 600 revolutions per minute, and then adding 0.5kg of carbon nano tube for continuous stirring for 30min.
b) Adding 80kg of silicone rubber and 7.5kg of epoxy resin into a), continuously stirring for 30min, then sequentially adding 80kg of silver-coated copper powder, 25kg of conductive zinc oxide (tetrapod-like) and 15kg of polyaniline, and continuously stirring for 60min;
c) Grinding: adjusting the distance between the front grinding roller and the rear grinding roller of the three-roller grinding machine, opening condensed water, starting the grinding machine, and enabling the rotating speed of the grinding machine to be 1000 revolutions per minute; adding the electromagnetic shielding adhesive after stirring in the step a) to the back roller of the regulated three-roller grinder for grinding, adding the electromagnetic shielding adhesive at the front roller discharge port of the three-roller grinder to the back roller for grinding after finishing grinding, repeatedly grinding for 4 times, and packaging after grinding to obtain an electromagnetic shielding adhesive A component;
c) Cleaning three rollers of the three-roller grinder by using gasoline, and closing condensed water and the three-roller grinder;
2) The preparation method of the electromagnetic shielding adhesive B comprises the following steps:
a) Weighing: 8kg of ethyl orthosilicate, 1.5kg of polyethylene polyamine, 0.3kg of organic tin dilaurate and 3.7kg of gasoline are weighed according to the formula ratio;
b) Stirring and dispersing: after weighing, adding tetraethoxysilane, polyethylene polyamine, organic tin dilaurate and gasoline into a pulling cylinder of a dispersing machine, starting the dispersing machine, absorbing, stirring and dispersing for 20min at the rotating speed of 600 revolutions per minute, and packaging after stirring and dispersing are finished to obtain a component B;
3) The electromagnetic shielding adhesive is prepared from an electromagnetic shielding adhesive A component and an electromagnetic shielding adhesive B component in a ratio of 100:7 when the electromagnetic shielding adhesive is to be constructed, and is cured for 96 hours at room temperature after an active period of 3 hours to be completely cured, so that the electromagnetic shielding adhesive is prepared.
The resistivity of the electromagnetic shielding glue prepared in example 3 is 2 multiplied by 10 -5 Omega.m, shielding effectiveness-22 dB (K wave), and bonding strength on polyurethane plastic of 2.7Mpa.
Example 4
4.1 high and low temperature resistant electromagnetic shielding adhesive is composed of the following formula ratio: the component A of the electromagnetic shielding adhesive and the component B of the electromagnetic shielding adhesive are 10:1;
4.2, the preparation method of the high-low temperature resistant electromagnetic shielding glue comprises the following steps:
1) The preparation method of the electromagnetic shielding adhesive A comprises the following steps:
a) Weighing, stirring and mixing: weighing 10kg of gasoline according to the formula ratio, adding 0.5kg of butyl titanate and 0.2kg of KYC913 into a dispersing agent drawing cylinder, absorbing, stirring and dispersing for 20min at the rotating speed of 600 revolutions per minute, and then adding 0.5kg of carbon nano tube for continuous stirring for 30min.
b) Adding 80kg of silicone rubber and 10kg of epoxy resin into a), continuously stirring for 30min, then sequentially adding 80kg of silver-coated copper powder, 25kg of conductive zinc oxide (tetrapod-like) and 15kg of polyaniline, and continuously stirring for 60min;
c) Grinding: adjusting the distance between the front grinding roller and the rear grinding roller of the three-roller grinding machine, opening condensed water, starting the grinding machine, and enabling the rotating speed of the grinding machine to be 1000 revolutions per minute; adding the electromagnetic shielding adhesive after stirring in the step a) to the back roller of the regulated three-roller grinder for grinding, adding the electromagnetic shielding adhesive at the front roller discharge port of the three-roller grinder to the back roller for grinding after finishing grinding, repeatedly grinding for 4 times, and packaging after grinding to obtain an electromagnetic shielding adhesive A component;
c) Cleaning three rollers of the three-roller grinder by using gasoline, and closing condensed water and the three-roller grinder;
2) The preparation method of the electromagnetic shielding adhesive B comprises the following steps:
a) Weighing: weighing 8kg of ethyl orthosilicate, 2kg of polyethylene polyamine, 0.3kg of organic tin dilaurate and 3.7kg of gasoline according to the formula ratio;
b) Stirring and dispersing: after weighing, adding tetraethoxysilane and gasoline into a pull cylinder in a dispersing machine, starting the dispersing machine, absorbing, stirring and dispersing for 20min at the rotating speed of 600 revolutions per minute, and packaging after stirring and dispersing are finished to obtain a component B;
4) The electromagnetic shielding adhesive is prepared from an electromagnetic shielding adhesive A component and an electromagnetic shielding adhesive B component in a ratio of 10:1 during construction, and is cured for 96 hours at room temperature to be completely cured, so that the electromagnetic shielding adhesive is prepared.
The resistivity of the electromagnetic shielding glue prepared in example 4 is 3.2X10 -5 Omega.m, shielding effectiveness-22 dB (K wave), and bonding strength on polyurethane easy plastic of 3.5Mpa.
1. Performance testing
The high and low temperature resistant electromagnetic shielding glue prepared in example 4 was subjected to performance test, and the results are shown in table 1.
Electromagnetic shielding glue main parameter test standard:
the tensile strength is carried out according to GB/T528-2009 "determination of tensile stress and strain properties of vulcanized rubber or thermoplastic rubber";
the elongation is carried out according to GB/T528-2009 "measurement of tensile stress and strain properties of vulcanized rubber or thermoplastic rubber";
the shearing strength at normal temperature is carried out according to GB7124-1986 adhesive tensile strength test method;
low temperature shear strength
Placing the electromagnetic shielding glue sample in the environments of-10 ℃, 20 ℃, 30 ℃ below zero and 45 ℃ below zero for 10min according to GB7124-1986 adhesive tensile strength test method;
high temperature shear Strength
Placing the electromagnetic shielding glue sample in environments of 100 ℃, 150 ℃, 200 ℃, 250 ℃ and 300 ℃ for 10min respectively, and then carrying out the process according to GB7124-1986 adhesive tensile strength test method;
shore hardness according to GB/T531-2009 method for testing indentation hardness of vulcanized rubber or thermoplastic rubber
The resistivity is carried out according to QJ1523-1988 method for testing resistivity of electromagnetic shielding adhesive;
low temperature resistivity
Placing the electromagnetic shielding glue sample in the environments of-10 ℃, 20 ℃, 30 ℃ below zero and 45 ℃ below zero for 10min respectively, and then carrying out the process according to QJ1523-1988 'electromagnetic shielding glue resistivity test method'; ,
high temperature resistivity
Placing the electromagnetic shielding glue sample in environments of 100 ℃, 150 ℃, 200 ℃, 250 ℃ and 300 ℃ for 10min respectively, and then carrying out the process according to QJ1523-1988 electromagnetic shielding glue resistivity test method;
isolation and phase sensitivity
The method is carried out according to the method specified in GJB17.6-1993 general Specification for missile antenna.
Shielding effectiveness
The method is carried out according to the method specified in GJB6190-2008 'method for measuring shielding effectiveness of electromagnetic shielding material'.
Table 1 comparison of technical indexes of the electromagnetic shielding adhesive with high and low temperature resistance according to the present invention and electromagnetic shielding adhesive with certain brand number
As can be seen from the data in Table 1, the high-low temperature resistant electromagnetic shielding adhesive has good shielding effectiveness, high-low temperature resistance, shearing strength and shearing strength at high temperature and room temperature which are higher than those of electromagnetic shielding adhesives of certain brands.
Table 2 electromagnetic shielding glue antenna isolation contrast
As can be seen from Table 2, the isolation of the electromagnetic shielding adhesive of the invention is higher than that of a certain brand of electromagnetic shielding adhesive when the antenna of different types is used.
Antenna full phase sensitivity after construction of electromagnetic shielding adhesive of certain brand number (Table 3) and antenna full phase sensitivity after construction of conductive adhesive of the invention (Table 4)
TABLE 3 antenna full phase sensitivity after construction of electromagnetic shielding adhesive of certain brand number
TABLE 4 full phase sensitivity of antennas after construction of electromagnetic shielding glue of the invention
TABLE 5 electromagnetic shielding glue with shielding effectiveness of electromagnetic shielding glue according to the invention
| Wave band | Certain brand electromagnetic shielding adhesive shielding effectiveness dB | The electromagnetic shielding adhesive of the invention has the shielding effectiveness dB |
| K | -13 | -22 |
As can be seen from tables 3 and 4, after the electromagnetic shielding glue of the present invention is used in the antenna, the antenna full-phase sensitivity values are lower than the antenna full-phase sensitivity after a certain brand is used in the antenna, and it is verified that the electromagnetic shielding glue of the present invention has better receiving performance after the antenna is used in the antenna than a certain brand, and the maximum variation of the antenna used in the electromagnetic shielding glue of the present invention is lower than the antenna used in a certain brand according to the variation calculation of the detected data, so that the electromagnetic shielding glue of the present invention is used in the antenna, and the antenna has stable sensitivity for receiving far targets, small variation and good overall effect. The data in the table 1 and the table 5 show that the electromagnetic shielding glue developed by the invention has stronger bonding strength and shielding effectiveness on polyurethane plastics. The glue solution is diluted by a solvent and is applied to a fragile cover of a transmitting cylinder made of polyurethane foam plastic in a spraying mode, so that a uniform shielding coating with a certain thickness is formed, and the shielding effect on a specific wave band is good.
The invention develops the novel high-low temperature resistant electromagnetic shielding adhesive with high shielding effectiveness, wide use temperature range and easy reverse operation construction, so as to realize shortening of the production period of the product, reduction of the production cost and controllable technology, and replace the application of a certain brand of high temperature resistant conductive shielding silicone rubber on model products. The high-low temperature resistant electromagnetic shielding glue provided by the invention meets the technical standards and application requirements under complex conditions.
Claims (6)
1. The high-low temperature resistant electromagnetic shielding adhesive is characterized by comprising the following components in percentage by mass: the component A of the electromagnetic shielding adhesive and the component B of the electromagnetic shielding adhesive are 10:1;
the electromagnetic shielding adhesive A comprises the following raw materials in parts by weight:
80-100 parts of silicon rubber, 0-20 parts of epoxy resin, 0-15 parts of polyaniline, 80-100 parts of silver-coated copper powder, 0-1 part of carbon nano tube, 15-35 parts of zinc oxide, 10-50 parts of gasoline, 0.2-0.5 part of butyl titanate and 0.2-0.5 part of KYC 913;
the electromagnetic shielding adhesive B component consists of the following raw materials in parts by weight:
4 to 8 parts of tetraethoxysilane, 10 to 20 parts of polyethylene polyamine, 0.1 to 0.3 part of organic tin and 1.2 to 3.7 parts of gasoline.
2. The method for preparing the high and low temperature resistant electromagnetic shielding glue according to claim 1, comprising the following steps:
1) And (3) preparing an electromagnetic shielding adhesive A component:
a) Weighing, stirring and mixing: weighing silicon rubber, epoxy resin, polyaniline, silver-coated copper powder, carbon nano tubes, zinc oxide and butyl titanate according to the formula ratio, placing gasoline into a pulling cylinder of a dispersing machine, and starting the dispersing machine to stir;
b) Grinding: adjusting the distance between the front grinding roller and the rear grinding roller of the three-roller grinding machine, opening condensed water, starting the grinding machine, and enabling the rotating speed of the grinding machine to be 1000 revolutions per minute; adding the electromagnetic shielding adhesive after stirring in the step a) at the rear roller of the regulated three-roller grinder for grinding, adding the electromagnetic shielding adhesive at the front roller discharge port of the three-roller grinder to the rear roller for grinding after finishing grinding, and packaging after finishing grinding to obtain an electromagnetic shielding adhesive component A;
2) And (3) preparing an electromagnetic shielding adhesive B component:
a) Weighing: weighing tetraethoxysilane, polyethylene polyamine, organic tin and gasoline according to the formula ratio;
b) Stirring and dispersing: adding tetraethoxysilane, polyethylene polyamine, organic tin and gasoline into a pulling cylinder of a dispersing machine, starting the dispersing machine, and packaging after stirring and dispersing are finished to obtain a component B;
3) During construction, the component A and the component B of the electromagnetic shielding adhesive are prepared according to the proportion of 10:1, and are cured for 96 hours at room temperature.
3. The method for preparing the high-low temperature resistant electromagnetic shielding glue as claimed in claim 2, wherein the method comprises the following steps: the silicone rubber is methyl diphenyl sulfide silicone rubber; the polyaniline is conductive polyaniline; the zinc oxide is conductive zinc oxide with a tetrapod structure; the silver-coated copper powder is of a sheet structure, and the silver content of the copper powder is 10%; the carbon nano tube is a multi-wall carbon nano tube; the organic tin is butyl tin dilaurate.
4. The method for preparing a high and low temperature resistant electromagnetic shielding glue according to claim 2, wherein in step 1), the stirring in step a) is performed at 600 rpm for 30min.
5. The method for preparing the high and low temperature resistant electromagnetic shielding adhesive according to claim 2, wherein in the step 1), the grinding in the step c) is performed, the electromagnetic shielding adhesive in the step a) is added at the rear roller of the three-roller grinder for grinding, and after the grinding is finished, the electromagnetic shielding adhesive at the front roller discharge port of the three-roller grinder is added at the rear roller for grinding, and the grinding is repeatedly performed for 4 times.
6. The method for preparing a high and low temperature resistant electromagnetic shielding glue according to claim 2, wherein in step 2), the stirring and dispersing in step b) are performed, and the stirring and dispersing are performed at a rotation speed of 600 rpm for 20min.
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