CN113402840B - Electromagnetic interference resistant shielding material for visibility meter and preparation method thereof - Google Patents
Electromagnetic interference resistant shielding material for visibility meter and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of polymer composite materials, in particular to an anti-electromagnetic interference shielding material for a visibility meter and a preparation method thereof, wherein the shielding material comprises the following components: tests prove that the shielding material prepared by the invention has good mechanical property and salt corrosion resistance and has good electromagnetic shielding effectiveness under 150kHz-18GHz, wherein the shielding effectiveness of the material under 150kHz-30MHz is more than or equal to 40dB, and the shielding effectiveness under 450MHz-18GHz is more than or equal to 70 dB.
Description
Technical Field
The invention relates to the field of polymer composite materials, in particular to an anti-electromagnetic interference shielding material for a visibility meter and a preparation method thereof.
Background
The visibility meter is an instrument for measuring atmospheric visibility distance, and can generate a lot of adverse effects on transportation and power supply of ships, civil aviation, highways and the like due to low visibility so that the daily life of citizens can be caused.
The visibility meter is generally subjected to electromagnetic interference in the using process, so that the normal work of the visibility meter is influenced, and the visibility meter is generally made of an electromagnetic shielding material made of a metal material in the market at present. The shielding mode is mainly reflection loss, and the absorption loss is very small or none, so that the main advantages are as follows: the electromagnetic shielding material has the advantages of high strength, good toughness, good electric conduction, magnetic conduction and heat conduction performance and high shielding efficiency, and has good shielding performance and excellent corrosion resistance aiming at complicated and various electromagnetic interference of an visibility meter on a ship and severe operating environments with large humidity and salinity, and the electromagnetic shielding material of a metal material is difficult to meet the use requirement.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the defects or the improvement requirement of the prior art, the invention provides an anti-electromagnetic interference shielding material for a visibility meter and a preparation method thereof.
The technical scheme adopted by the invention is as follows:
an anti-electromagnetic interference shielding material for a visibility meter comprises the following components:
ABS, polycarbonate, polybutylene terephthalate, SMA resin, ABS-g-MAH, styrene-acrylonitrile-glycidyl methacrylate, a dispersant PETS, microcrystalline paraffin, hollow tubular nickel/carbon nanotube/nickel composite fiber, an antioxidant and a flame retardant HT-102.
Further, the feed additive comprises the following components in parts by weight:
50-60 parts of ABS, 30-35 parts of polycarbonate, 5-10 parts of polybutylene terephthalate, 5-10 parts of SMA resin, 1-3 parts of ABS-g-MAH, 0.1-1 part of styrene-acrylonitrile-glycidyl methacrylate, 0.1-0.5 part of dispersant PETS, 1-2 parts of microcrystalline paraffin, 5-10 parts of hollow tubular nickel/carbon nanotube/nickel composite fiber, 0.1-0.5 part of antioxidant and 0.5 part of flame retardant HT-1020.1.
Furthermore, the composition comprises the following components in parts by weight:
60 parts of ABS, 35 parts of polycarbonate, 10 parts of polybutylene terephthalate, 8 parts of SMA resin, 2 parts of ABS-g-MAH, 0.5 part of styrene-acrylonitrile-glycidyl methacrylate, 0.1 part of dispersant PETS, 1.5 parts of microcrystalline paraffin, 10 parts of hollow tubular nickel/carbon nanotube/nickel composite fiber, 0.1 part of antioxidant and HT-1020.1 parts of flame retardant.
Further, the preparation method of the hollow tubular nickel/carbon nanotube/nickel composite fiber comprises the following steps:
taking PVC nano-fiber as a sacrificial template, plating nickel on the surface of the PVC fiber, then immersing the PVC nano-fiber in THF to remove the PVC nano-fiber to obtain a nano-nickel tube, depositing a carbon nano-tube layer on the nano-nickel tube by using a chemical vapor deposition method, and finally plating nickel on the surface of the nano-tube layer to obtain the hollow tubular nickel/carbon nano-tube/nickel composite fiber.
Generally speaking, carbon nanotubes themselves have no catalytic activity, and metal nickel is difficult to deposit directly on the carbon nanotubes, and after experiments, the inventor finds that if the purchased carbon nanotubes are directly used, the metal nickel is difficult to deposit, but the carbon nanotube layer deposited by the chemical vapor deposition method does not have the problem, which may be the influence of a high-temperature environment and a residual catalyst, and improves the surface activity of the carbon nanotube layer, so that the metal nickel can be deposited on the carbon nanotubes.
Furthermore, the preparation method of the hollow tubular nickel/carbon nanotube/nickel composite fiber comprises the following specific steps:
s1: preparing PVC nano-fiber by using an electrostatic spinning method, immersing the PVC nano-fiber into nickel plating solution, adding metal powder with electrode potential lower than nickel, adjusting the temperature of the nickel plating solution to 50-60 ℃, performing ultrasonic oscillation and stirring for 120min, taking out, performing vacuum drying, immersing into THF, heating to reflux and stirring for 50-100min, taking out, and performing vacuum drying to obtain a nano-nickel tube;
s2: soaking the nano nickel tube into the catalyst solution for 5-10s, taking out, vacuum drying, and placing in chemical vapor deposition equipment, wherein N is2Raising the temperature to 750 ℃ and 950 ℃ under protection, and introducing CH4And N2/H2Reacting the mixed gas for 40-80min, and reacting with N2Recovering the temperature to room temperature under protection, and taking out;
in the step, the surface of the nano nickel tube deposited with the carbon nano tube may still have residual catalyst or amorphous carbon, and the catalyst or amorphous carbon can be purified by acid liquor treatment.
S3: and (2) immersing the nano nickel tube deposited with the carbon nano tube into nickel plating solution, adding metal powder with the electrode potential lower than that of nickel, adjusting the temperature of the nickel plating solution to 50-60 ℃, performing ultrasonic oscillation and stirring for 120min, taking out, and performing vacuum drying to obtain the hollow tubular nickel/carbon nano tube/nickel composite fiber.
Further, the nickel plating solution comprises the following components in parts by weight:
20-30g/L of nickel sulfate, 30-35g/L of sodium hypophosphite, 5-10g/L of sodium citrate, 30-35g/L of ammonium chloride, 0.2-0.5g/L of succinic acid, adding 1L of water, and adjusting the pH value to 8.5-9.5 by ammonia water.
Further, the metal powder is iron powder or aluminum powder.
Further, the catalyst solution consists of the following components in parts by weight:
10-20 parts of magnesium nitrate, 10-20 parts of nickel nitrate, 40-50 parts of ammonium molybdate and 150 parts of ethylene glycol 100-.
Further, the antioxidant is prepared from an antioxidant 1010 and an antioxidant 168 according to a mass ratio of 1-5: 1-5.
The preparation method of the anti-electromagnetic interference shielding material for the visibility meter comprises the following steps:
the raw materials are dried and then uniformly mixed in a high-speed mixer, and then are added into a double-screw extruder for extrusion granulation, the rotating speed of a main machine screw of the double-screw extruder is 180 plus 200r/min, the temperatures of all sections are 210 plus 215 ℃, 230 plus 235 ℃, 240 plus 245 ℃ and 250 plus 255 ℃, and the obtained granules are dried at 90-95 ℃ for 6-10h and then injection molding is carried out at 260 ℃ by an injection molding machine.
The basic principle of electromagnetic shielding is as follows: the low-resistance conductor material is adopted, and the electromagnetic wave emission on the surface of the shielding conductor, the absorption in the conductor and the loss in the transmission process are utilized to prevent the electromagnetic wave energy from being transmitted continuously, thereby playing the role of shielding. That is, the shielding body shields the far-zone field of the radiation interference source by emission and absorption of electromagnetic waves, and simultaneously shields the electric field and the magnetic field components generated by the field source.
Electromagnetic shielding means shielding both electric and magnetic fields, and we generally refer to shielding effectiveness, which is defined as: in the presence of shielding, the ratio of the absolute value of the electric field (magnetic field) at a certain point to the absolute value of the electric field (magnetic field) at that point in the unshielded state is expressed in decibels (dB). For interference sources with lower frequency, the shielding effectiveness of the magnetic field is often smaller than that of the electric field, and the shielding effectiveness SE of the shielding material on the magnetic field is mainly considered when performing electromagnetic shielding analysisH. The empirical formula of the magnetic shielding effectiveness of the material can be derived by using the transmission line theory:
SEH＝Rm+A+Rr；
in the formula: f is frequency, Hz; μ r is the relative permeability of the shielding material; gr is the conductivity of the shielding material relative to copper; r represents the distance, cm, of the shield plate from the source; t represents the thickness of the shielding plate, mm; zmThe impedance of the conductor used for the shield, Ω; zwIs the wave impedance, Ω;
for magnetic fields, when r < λ/2 π, the wave impedance can be expressed as:
Zw＝377*2πr/λ
in the formula: r is the distance between the shield and the source, λ is the wavelength, m;
the impedance of a metal conductor can be expressed as:
Zm＝(wμo/2σ)1/2*(1+j)
in the formula: w is the angular frequency; mu.soIs a vacuum magnetic conductivity; σ is the shield material conductivity.
According to the six formulas, the magnetic field shielding effect depends on the thickness t of the shielding body, the relative conductivity sigma and the relative permeability mu of the shielding materialrAnd the distance r of the interference source from the shield.
The shielding material with high magnetic conductivity and high electric conductivity can effectively improve the shielding efficiency on low-frequency interference.
The invention has the beneficial effects that:
the invention provides an anti-electromagnetic interference shielding material for visibility meter, wherein ABS is a tough, hard and rigid material with easily obtained raw materials, good comprehensive performance, low price and wide application, after being compounded with polycarbonate, the ABS can reduce melt viscosity, improve fluidity, improve processing performance and reduce internal stress of products, the addition of polybutylene terephthalate can improve thermal deformation temperature, corrosion resistance, wear resistance, dimensional stability and stress cracking resistance, SMA resin, ABS-g-MAH and styrene-acrylonitrile-glycidyl methacrylate are taken as compatilizers, the bonding performance and dispersion performance among material components can be improved, the effects of reducing phase interface tension, improving interphase compatibility and binding power are achieved, the hollow tubular nickel/carbon nanotube/nickel composite fiber has higher magnetic conductivity and electrical conductivity, according to the GB/T351-1995 and GB/T13012-2008 standards, the relative conductivity is not less than 0.83, the relative magnetic conductivity is not less than 580, and the electromagnetic protection function is good, and through tests, the shielding material prepared by the invention has good mechanical property and salt corrosion resistance, and has good electromagnetic shielding effectiveness under 150kHz-18GHz, wherein the shielding effectiveness of the material under 150kHz-30MHz is not less than 40dB, and the shielding effectiveness under 450MHz-18GHz is not less than 70 dB.
Detailed Description
The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1:
an anti-electromagnetic interference shielding material for a visibility meter comprises the following components in parts by weight:
60 parts of ABS, 35 parts of polycarbonate, 10 parts of polybutylene terephthalate, 8 parts of SMA resin, 2 parts of ABS-g-MAH, 0.5 part of styrene-acrylonitrile-glycidyl methacrylate, 0.1 part of dispersant PETS, 1.5 parts of microcrystalline paraffin, 10 parts of hollow tubular nickel/carbon nanotube/nickel composite fiber, 1010 parts of antioxidant and 168 parts of antioxidant in a mass ratio of 1: 1 and 0.1 part of antioxidant and HT-1020.1 parts of flame retardant.
The preparation method of the hollow tubular nickel/carbon nanotube/nickel composite fiber comprises the following steps:
preparing PVC nano-fibers by using an electrostatic spinning method, and immersing the PVC nano-fibers into a nickel plating solution, wherein the nickel plating solution comprises the following components in parts by weight: 30g/L of nickel sulfate, 30g/L of sodium hypophosphite, 5g/L of sodium citrate, 30g/L of ammonium chloride, 0.5g/L of succinic acid, 1L of water and 1L of ammonia water for regulating the pH value to 9.5, meanwhile, adding iron powder for catalysis, regulating the temperature of the nickel plating solution to 50 ℃, ultrasonically oscillating and stirring for 100min, then taking out, vacuum drying, then immersing in THF, heating to reflux and stirring for 80min, then taking out, vacuum drying to obtain a nano nickel tube, immersing the nano nickel tube in a catalyst solution for 10s, then taking out and vacuum drying, wherein the catalyst solution consists of the following components in parts by weight: 15 parts of magnesium nitrate, 10 parts of nickel nitrate, 40 parts of ammonium molybdate and 120 parts of ethylene glycol, and then placing the mixture in chemical vapor deposition equipment, wherein N is2Raising the temperature to 900 ℃ under protection, and introducing CH4And 80% N2/20％H2Mixed gas, CH4Flow rate 15mL/min, 80% N2/20％H2The flow rate of the mixed gas is 10mL/min, after 50min of reaction, N2Recovering to room temperature under protection, taking out, and depositing carbon nanotubeThe nano nickel tube is immersed into the nickel plating solution, the temperature of the nickel plating solution is adjusted to 50 ℃ under the catalysis of iron powder, the nano nickel tube is taken out after ultrasonic oscillation and stirring for 100min, and the hollow tubular nickel/carbon nano tube/nickel composite fiber can be obtained after vacuum drying.
The preparation method of the anti-electromagnetic interference shielding material for the visibility meter comprises the following steps:
drying the raw materials, uniformly mixing in a high-speed mixer, adding into a double-screw extruder, extruding and granulating, wherein the rotation speed of a main machine screw of the double-screw extruder is 200r/min, the temperatures of all sections are 210 ℃, 230 ℃, 240 ℃ and 255 ℃ in sequence, drying the obtained granules at 90 ℃ for 10h, and then performing injection molding at 250 ℃ by using an injection molding machine.
Example 2:
an anti-electromagnetic interference shielding material for a visibility meter comprises the following components in parts by weight:
50 parts of ABS, 30 parts of polycarbonate, 5 parts of polybutylene terephthalate, 5 parts of SMA resin, 1 part of ABS-g-MAH, 0.5 part of styrene-acrylonitrile-glycidyl methacrylate, 0.1 part of dispersant PETS, 1 part of microcrystalline paraffin, 8 parts of hollow tubular nickel/carbon nano tube/nickel composite fiber, 1010 parts of antioxidant and 168 parts of antioxidant in a mass ratio of 2: 1 and 0.1 part of antioxidant and HT-1020.5 parts of flame retardant.
The preparation method of the hollow tubular nickel/carbon nanotube/nickel composite fiber comprises the following steps:
preparing PVC nano-fibers by using an electrostatic spinning method, and immersing the PVC nano-fibers into a nickel plating solution, wherein the nickel plating solution comprises the following components in parts by weight: 20g/L of nickel sulfate, 30g/L of sodium hypophosphite, 5g/L of sodium citrate, 32g/L of ammonium chloride, 0.4g/L of succinic acid, 1L of water and 1L of ammonia water for regulating the pH value to 9.5, meanwhile, adding iron powder for catalysis, regulating the temperature of a nickel plating solution to 60 ℃, ultrasonically oscillating and stirring for 120min, then taking out, vacuum drying, then immersing in THF, heating to reflux and stirring for 100min, then taking out, vacuum drying to obtain a nano nickel tube, immersing the nano nickel tube in a catalyst solution for 5s, then taking out and vacuum drying, wherein the catalyst solution consists of the following components in parts by weight: 20 parts of magnesium nitrate, 12 parts of nickel nitrate, 45 parts of ammonium molybdate and 100 parts of ethylene glycol, and then placing the mixture into a chemical reactorIn a vapor deposition apparatus, N2Raising the temperature to 950 ℃ under protection, and introducing CH4And 80% N2/20％H2Mixed gas, CH4Flow rate 20mL/min, 80% N2/20％H2The flow rate of the mixed gas is 10mL/min, and N is obtained after the reaction is carried out for 60min2And (2) recovering the temperature to room temperature under protection, taking out, immersing the nano nickel tube deposited with the carbon nano tube into the nickel plating solution, catalyzing by iron powder, adjusting the temperature of the nickel plating solution to 60 ℃, ultrasonically oscillating, stirring for 120min, taking out, and drying in vacuum to obtain the hollow tubular nickel/carbon nano tube/nickel composite fiber.
The preparation method of the anti-electromagnetic interference shielding material for the visibility meter comprises the following steps:
drying the raw materials, uniformly mixing in a high-speed mixer, adding into a double-screw extruder, extruding and granulating, wherein the rotating speed of a main machine screw of the double-screw extruder is 200r/min, the temperatures of all sections are 215 ℃, 230 ℃, 245 ℃ and 250 ℃, the obtained granules are dried for 10 hours at 90 ℃ and then injection molding is carried out at 250 ℃ by an injection molding machine.
Example 3:
an anti-electromagnetic interference shielding material for a visibility meter comprises the following components in parts by weight:
50 parts of ABS, 30 parts of polycarbonate, 5 parts of polybutylene terephthalate, 5 parts of SMA resin, 1 part of ABS-g-MAH, 0.1 part of styrene-acrylonitrile-glycidyl methacrylate, 0.1 part of dispersant PETS, 1 part of microcrystalline paraffin, 5 parts of hollow tubular nickel/carbon nano tube/nickel composite fiber, 1010 antioxidant and 168 parts by mass in a ratio of 1: 1 and 0.1 part of antioxidant and HT-1020.1 parts of flame retardant.
The preparation method of the hollow tubular nickel/carbon nanotube/nickel composite fiber comprises the following steps:
preparing PVC nano-fibers by using an electrostatic spinning method, and immersing the PVC nano-fibers into a nickel plating solution, wherein the nickel plating solution comprises the following components in parts by weight: nickel sulfate 20g/L, sodium hypophosphite 30g/L, sodium citrate 5g/L, ammonium chloride 30g/L, succinic acid 0.2g/L, water 1L, ammonia water pH 8.5, adding iron powder for catalysis, adjusting nickel plating solution temperature to 50 deg.C, ultrasonic oscillating and stirringStirring for 100min, taking out, vacuum drying, immersing in THF, heating to reflux, stirring for 50min, taking out, vacuum drying to obtain a nano nickel tube, immersing the nano nickel tube in a catalyst solution for 5s, taking out, vacuum drying, wherein the catalyst solution comprises the following components in parts by weight: 10 parts of magnesium nitrate, 10 parts of nickel nitrate, 40 parts of ammonium molybdate and 100 parts of ethylene glycol, and then placing the mixture in chemical vapor deposition equipment, wherein N is2Raising the temperature to 750 ℃ under protection, and introducing CH4And 80% N2/20％H2Mixed gas, CH4Flow rate 10mL/min, 80% N2/20％H2The flow rate of the mixed gas is 10mL/min, after 40min of reaction, N2And (2) recovering the temperature to room temperature under protection, taking out, immersing the nano nickel tube deposited with the carbon nano tube into the nickel plating solution, catalyzing by iron powder, adjusting the temperature of the nickel plating solution to 50 ℃, ultrasonically oscillating, stirring for 100min, taking out, and drying in vacuum to obtain the hollow tubular nickel/carbon nano tube/nickel composite fiber.
The preparation method of the anti-electromagnetic interference shielding material for the visibility meter comprises the following steps:
drying the raw materials, uniformly mixing in a high-speed mixer, adding into a double-screw extruder, extruding and granulating, wherein the rotating speed of a main machine screw of the double-screw extruder is 180r/min, the temperatures of all sections are 210 ℃, 230 ℃, 240 ℃ and 250 ℃ in sequence, drying the obtained granules at 90 ℃ for 6h, and then performing injection molding at 240 ℃ by an injection molding machine.
Example 4:
an anti-electromagnetic interference shielding material for a visibility meter comprises the following components in parts by weight:
60 parts of ABS, 35 parts of polycarbonate, 10 parts of polybutylene terephthalate, 10 parts of SMA resin, 3 parts of ABS-g-MAH, 1 part of styrene-acrylonitrile-glycidyl methacrylate, 0.5 part of dispersant PETS, 2 parts of microcrystalline paraffin, 10 parts of hollow tubular nickel/carbon nanotube/nickel composite fiber, 1010 parts of antioxidant and 168 parts of antioxidant in a mass ratio of 5: 1 and 0.5 part of antioxidant and HT-1020.5 parts of flame retardant.
The preparation method of the hollow tubular nickel/carbon nanotube/nickel composite fiber comprises the following steps:
by usingPreparing PVC nano-fiber by an electrostatic spinning method, and immersing the PVC nano-fiber into a nickel plating solution, wherein the nickel plating solution comprises the following components in parts by weight: 30g/L of nickel sulfate, 35g/L of sodium hypophosphite, 10g/L of sodium citrate, 35g/L of ammonium chloride, 0.5g/L of succinic acid, 1L of water and ammonia water for regulating the pH value to 9.5, meanwhile, adding iron powder for catalysis, regulating the temperature of a nickel plating solution to 60 ℃, ultrasonically oscillating and stirring for 120min, then taking out, vacuum drying, then immersing in THF, heating to reflux and stirring for 100min, then taking out, vacuum drying to obtain a nano nickel tube, immersing the nano nickel tube in a catalyst solution for 10s, then taking out, and vacuum drying, wherein the catalyst solution consists of the following components in parts by weight: 20 parts of magnesium nitrate, 20 parts of nickel nitrate, 50 parts of ammonium molybdate and 150 parts of ethylene glycol, and then placing the mixture in chemical vapor deposition equipment, wherein N is2Raising the temperature to 950 ℃ under protection, and introducing CH4And 80% N2/20％H2Mixed gas, CH4Flow rate 20mL/min, 80% N2/20％H2The flow rate of the mixed gas is 10mL/min, after 80min of reaction, N2And (2) recovering the temperature to room temperature under protection, taking out, immersing the nano nickel tube deposited with the carbon nano tube into the nickel plating solution, catalyzing by iron powder, adjusting the temperature of the nickel plating solution to 60 ℃, ultrasonically oscillating, stirring for 120min, taking out, and drying in vacuum to obtain the hollow tubular nickel/carbon nano tube/nickel composite fiber.
The preparation method of the anti-electromagnetic interference shielding material for the visibility meter comprises the following steps:
drying the raw materials, uniformly mixing in a high-speed mixer, adding into a double-screw extruder, extruding and granulating, wherein the rotating speed of a main machine screw of the double-screw extruder is 200r/min, the temperatures of all sections are 215 ℃, 235 ℃, 245 ℃ and 255 ℃ in sequence, drying the obtained granules at 95 ℃ for 10h, and then performing injection molding at 260 ℃ by using an injection molding machine.
Example 5:
an anti-electromagnetic interference shielding material for a visibility meter comprises the following components in parts by weight:
50 parts of ABS, 35 parts of polycarbonate, 5 parts of polybutylene terephthalate, 10 parts of SMA resin, 1 part of ABS-g-MAH, 1 part of styrene-acrylonitrile-glycidyl methacrylate, 0.1 part of dispersant PETS, 2 parts of microcrystalline paraffin, 5 parts of hollow tubular nickel/carbon nanotube/nickel composite fiber, 1010 parts of antioxidant and 168 parts of antioxidant in a mass ratio of 5: 1 and 0.5 part of antioxidant and HT-1020.1 parts of flame retardant.
The preparation method of the hollow tubular nickel/carbon nanotube/nickel composite fiber comprises the following steps:
preparing PVC nano-fibers by using an electrostatic spinning method, and immersing the PVC nano-fibers into a nickel plating solution, wherein the nickel plating solution comprises the following components in parts by weight: 30g/L of nickel sulfate, 30g/L of sodium hypophosphite, 10g/L of sodium citrate, 30g/L of ammonium chloride, 0.5g/L of succinic acid, 1L of water and 1L of ammonia water for regulating the pH value to 8.5, meanwhile, adding iron powder for catalysis, regulating the temperature of the nickel plating solution to 50 ℃, ultrasonically oscillating and stirring for 120min, then taking out, vacuum drying, then immersing in THF, heating to reflux and stirring for 100min, then taking out, vacuum drying to obtain a nano nickel tube, immersing the nano nickel tube in a catalyst solution for 5s, then taking out and vacuum drying, wherein the catalyst solution consists of the following components in parts by weight: 20 parts of magnesium nitrate, 10 parts of nickel nitrate, 50 parts of ammonium molybdate and 100 parts of ethylene glycol, and then placing the mixture in chemical vapor deposition equipment, wherein N is2Raising the temperature to 950 ℃ under protection, and introducing CH4And 80% N2/20％H2Mixed gas, CH4Flow rate 10mL/min, 80% N2/20％H2The flow rate of the mixed gas is 10mL/min, after 80min of reaction, N2And (2) recovering the temperature to room temperature under protection, taking out, immersing the nano nickel tube deposited with the carbon nano tube into the nickel plating solution, catalyzing by iron powder, adjusting the temperature of the nickel plating solution to 50 ℃, ultrasonically oscillating, stirring for 120min, taking out, and drying in vacuum to obtain the hollow tubular nickel/carbon nano tube/nickel composite fiber.
The preparation method of the anti-electromagnetic interference shielding material for the visibility meter comprises the following steps:
drying the raw materials, uniformly mixing in a high-speed mixer, adding into a double-screw extruder, extruding and granulating, wherein the rotating speed of a main machine screw of the double-screw extruder is 180r/min, the temperatures of all sections are 215 ℃, 230 ℃, 245 ℃ and 250 ℃ in sequence, drying the obtained granules at 95 ℃ for 6 hours, and then performing injection molding at 260 ℃ by using an injection molding machine.
Example 6
An anti-electromagnetic interference shielding material for a visibility meter comprises the following components in parts by weight:
55 parts of ABS, 30 parts of polycarbonate, 10 parts of polybutylene terephthalate, 5 parts of SMA resin, 3 parts of ABS-g-MAH, 0.1 part of styrene-acrylonitrile-glycidyl methacrylate, 0.5 part of dispersant PETS, 1 part of microcrystalline paraffin, 10 parts of hollow tubular nickel/carbon nano tube/nickel composite fiber, 1010 parts of antioxidant and 168 parts of antioxidant in a mass ratio of 3: 1 and 0.1 part of antioxidant and HT-1020.5 parts of flame retardant.
The preparation method of the hollow tubular nickel/carbon nanotube/nickel composite fiber comprises the following steps:
preparing PVC nano-fibers by using an electrostatic spinning method, and immersing the PVC nano-fibers into a nickel plating solution, wherein the nickel plating solution comprises the following components in parts by weight: 20g/L of nickel sulfate, 35g/L of sodium hypophosphite, 5g/L of sodium citrate, 35g/L of ammonium chloride, 0.2g/L of succinic acid, 1L of water and 1L of ammonia water for regulating the pH value to 9.5, meanwhile, adding iron powder for catalysis, regulating the temperature of nickel plating solution to 50 ℃, ultrasonically oscillating and stirring for 120min, then taking out, vacuum drying, then immersing in THF, heating to reflux and stirring for 50min, then taking out, vacuum drying to obtain a nano nickel tube, immersing the nano nickel tube in a catalyst solution for 10s, then taking out and vacuum drying, wherein the catalyst solution consists of the following components in parts by weight: 10 parts of magnesium nitrate, 20 parts of nickel nitrate, 40 parts of ammonium molybdate and 150 parts of ethylene glycol, and then placing the mixture in chemical vapor deposition equipment, wherein N is2Raising the temperature to 750 ℃ under protection, and introducing CH4And 80% N2/20％H2Mixed gas, CH4Flow rate 20mL/min, 80% N2/20％H2The flow rate of the mixed gas is 10mL/min, after 40min of reaction, N2And (2) recovering the temperature to room temperature under protection, taking out, immersing the nano nickel tube deposited with the carbon nano tube into the nickel plating solution, catalyzing by iron powder, adjusting the temperature of the nickel plating solution to 60 ℃, ultrasonically oscillating, stirring for 100min, taking out, and drying in vacuum to obtain the hollow tubular nickel/carbon nano tube/nickel composite fiber.
The preparation method of the anti-electromagnetic interference shielding material for the visibility meter comprises the following steps:
drying the raw materials, uniformly mixing in a high-speed mixer, adding into a double-screw extruder, extruding and granulating, wherein the rotating speed of a main machine screw of the double-screw extruder is 200r/min, the temperatures of all sections are 210 ℃, 235 ℃, 245 ℃ and 255 ℃, the obtained granules are dried for 10 hours at 90 ℃ and then injection molding is carried out at 250 ℃ by an injection molding machine.
Comparative example 1
Comparative example 1 is substantially the same as example 1 except that a nickel-plated carbon fiber (manufacturer: boomerang) is used in place of the hollow tubular nickel/carbon nanotube/nickel composite fiber.
Comparative example 2
Comparative example 2 is substantially the same as example 1 except that the hollow tubular nickel/carbon nanotube/nickel composite fiber was replaced with nickel-plated carbon nanotubes (manufacturer: gold, germany).
And (3) performance testing:
test (1)
The impact strength of the cantilever beam notch is measured according to GB/T1843-2008, and the notch is a V-shaped notch with an angle of 45 degrees;
tensile properties were determined according to GB/T1040-2006;
the bending properties were determined according to GB/T1042-79;
MFR is determined according to GB/T3682-2000, and the test condition is 220 ℃ and 10 kg;
the vertical burning performance is measured according to UL94-2000, and the thickness is 1.6 mm;
LOI was determined according to GB/T2406.2-2009;
the results of the performance tests are shown in table 1 below:
TABLE 1
Test 2
The electromagnetic shielding effectiveness (dB) was measured at 150kHz-18GHz according to GB12190-2006, and the results are shown in Table 2:
table 2:
| 150kHz | 30MHz | 450MHz | 1GHz | 10GHz | 18GHz | |
| example 1 | 45 | 58 | 73 | 88 | 86 | 75 |
| Example 2 | 42 | 55 | 74 | 82 | 86 | 71 |
| Example 3 | 45 | 53 | 70 | 85 | 82 | 73 |
| Example 4 | 44 | 56 | 73 | 76 | 80 | 70 |
| Example 5 | 40 | 55 | 73 | 80 | 85 | 70 |
| Example 6 | 43 | 52 | 71 | 87 | 84 | 71 |
| Comparative example 1 | 33 | 37 | 62 | 70 | 72 | 58 |
| Comparative example 2 | 35 | 41 | 63 | 72 | 75 | 63 |
Test (c)
The salt corrosion resistance is measured according to GB/T1690-2010, the dumbbell-shaped test sample is immersed in a sodium chloride hydrothermal reaction kettle with the mass fraction of 10% for 24 hours at 40 ℃, and is taken out of an electric heating constant temperature blast drying oven at 100 ℃ for 24 hours for mechanical property test.
The test results are shown in table 3 below ("+" is an increase "-" is a decrease):
table 3:
the test shows that the shielding material prepared by the invention has good mechanical property and salt corrosion resistance, and has good electromagnetic shielding effectiveness under 150kHz-18 GHz.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. An anti-electromagnetic interference shielding material for a visibility meter is characterized by comprising the following components:
ABS, polycarbonate, polybutylene terephthalate, SMA resin, ABS-g-MAH, styrene-acrylonitrile-glycidyl methacrylate, a dispersant PETS, microcrystalline paraffin, hollow tubular nickel/carbon nanotube/nickel composite fiber, an antioxidant and a flame retardant HT-102;
the preparation method of the hollow tubular nickel/carbon nanotube/nickel composite fiber comprises the following steps:
taking PVC nano-fiber as a sacrificial template, plating nickel on the surface of the PVC nano-fiber, then immersing the PVC nano-fiber in THF to remove the PVC nano-fiber to obtain a nano-nickel tube, depositing a carbon nano-tube layer on the nano-nickel tube by using a chemical vapor deposition method, and finally plating nickel on the surface of the nano-tube layer to obtain the hollow tubular nickel/carbon nano-tube/nickel composite fiber.
2. The electromagnetic interference resistant shielding material for the visibility meter according to claim 1, which is composed of the following components in parts by weight:
50-60 parts of ABS, 30-35 parts of polycarbonate, 5-10 parts of polybutylene terephthalate, 5-10 parts of SMA resin, 1-3 parts of ABS-g-MAH, 0.1-1 part of styrene-acrylonitrile-glycidyl methacrylate, 0.1-0.5 part of dispersant PETS, 1-2 parts of microcrystalline paraffin, 5-10 parts of hollow tubular nickel/carbon nanotube/nickel composite fiber, 0.1-0.5 part of antioxidant and 0.5 part of flame retardant HT-1020.1.
3. The electromagnetic interference resistant shielding material for the visibility meter according to claim 1, which is composed of the following components in parts by weight:
60 parts of ABS, 35 parts of polycarbonate, 10 parts of polybutylene terephthalate, 8 parts of SMA resin, 2 parts of ABS-g-MAH, 0.5 part of styrene-acrylonitrile-glycidyl methacrylate, 0.1 part of dispersant PETS, 1.5 parts of microcrystalline paraffin, 10 parts of hollow tubular nickel/carbon nanotube/nickel composite fiber, 0.1 part of antioxidant and HT-1020.1 parts of flame retardant.
4. The electromagnetic interference resistant shielding material for the visibility meter according to claim 1, wherein the hollow tubular nickel/carbon nanotube/nickel composite fiber is prepared by a method comprising:
s1: preparing PVC nano-fiber by using an electrostatic spinning method, immersing the PVC nano-fiber into nickel plating solution, adding metal powder with electrode potential lower than nickel, adjusting the temperature of the nickel plating solution to 50-60 ℃, performing ultrasonic oscillation and stirring for 120min, taking out, performing vacuum drying, immersing into THF, heating to reflux and stirring for 50-100min, taking out, and performing vacuum drying to obtain a nano-nickel tube;
s2: soaking the nano nickel tube into the catalyst solution for 5-10s, taking out, vacuum drying, and placing in chemical vapor deposition equipment, wherein N is2Raising the temperature to 750 ℃ and 950 ℃ under protection, and introducing CH4And N2/H2Reacting the mixed gas for 40-80min, and reacting with N2Recovering the temperature to room temperature under protection, and taking out;
s3: and (2) immersing the nano nickel tube deposited with the carbon nano tube into nickel plating solution, adding metal powder with the electrode potential lower than that of nickel, adjusting the temperature of the nickel plating solution to 50-60 ℃, performing ultrasonic oscillation and stirring for 120min, taking out, and performing vacuum drying to obtain the hollow tubular nickel/carbon nano tube/nickel composite fiber.
5. The electromagnetic interference resistant shielding material for the visibility meter according to claim 4, wherein the nickel plating solution comprises the following components in parts by weight:
20-30g/L of nickel sulfate, 30-35g/L of sodium hypophosphite, 5-10g/L of sodium citrate, 30-35g/L of ammonium chloride, 0.2-0.5g/L of succinic acid, adding 1L of water, and adjusting the pH value to 8.5-9.5 by ammonia water.
6. The electromagnetic interference shielding material for the visibility meter according to claim 4, wherein the metal powder is iron powder or aluminum powder.
7. The electromagnetic interference resistant shielding material for the visibility meter according to claim 4, wherein the catalyst solution comprises the following components in parts by weight:
10-20 parts of magnesium nitrate, 10-20 parts of nickel nitrate, 40-50 parts of ammonium molybdate and 150 parts of ethylene glycol 100-.
8. The electromagnetic interference resistant shielding material for the visibility meter according to claim 1, wherein the antioxidant is prepared from antioxidant 1010 and antioxidant 168 according to a mass ratio of 1-5: 1-5.
9. The preparation method of the electromagnetic interference resistant shielding material for the visibility meter as claimed in any one of claims 1 to 8, characterized in that the raw materials are dried and then uniformly mixed in a high-speed mixer, and then the mixture is added into a twin-screw extruder for extrusion and granulation, the rotation speed of a main machine screw of the twin-screw extruder is 180-.
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Denomination of invention: A shielding material with electromagnetic interference resistance for visibility meter and its preparation method Effective date of registration: 20221027 Granted publication date: 20220415 Pledgee: Hunan Xiangjiang Zhongying Investment Management Co.,Ltd. Pledgor: HUNAN GUOTIAN ELECTRONIC TECHNOLOGY CO.,LTD. Registration number: Y2022980019937 |
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