CN112301733B - Preparation method of three-dimensional light-weight structural composite electromagnetic shielding material - Google Patents

Preparation method of three-dimensional light-weight structural composite electromagnetic shielding material Download PDF

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CN112301733B
CN112301733B CN202011117428.6A CN202011117428A CN112301733B CN 112301733 B CN112301733 B CN 112301733B CN 202011117428 A CN202011117428 A CN 202011117428A CN 112301733 B CN112301733 B CN 112301733B
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absorbing
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molecular sieve
wave
electromagnetic shielding
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CN112301733A (en
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陈美玉
来悦
李利娜
孙润军
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Xian Polytechnic University
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/28—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F6/30—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds comprising olefins as the major constituent
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00—Screening of apparatus or components against electric or magnetic fields
    • H05K9/0073—Shielding materials
    • H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
    • H05K9/0084—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising a single continuous metallic layer on an electrically insulating supporting structure, e.g. metal foil, film, plating coating, electro-deposition, vapour-deposition
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00—Screening of apparatus or components against electric or magnetic fields
    • H05K9/0073—Shielding materials
    • H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
    • H05K9/009—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive fibres, e.g. metal fibres, carbon fibres, metallised textile fibres, electro-conductive mesh, woven, non-woven mat, fleece, cross-linked
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32—Polyesters
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/34—Polyamides

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  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
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  • Manufacturing & Machinery (AREA)
  • Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)

Abstract

The invention discloses a preparation method of a three-dimensional light structure type composite electromagnetic shielding material, which comprises the following steps: mixing nano Fe 3 O 4 Carrying out hydrophilic modification on the powder, preparing a nano-encapsulated molecular sieve by adopting a layer-by-layer assembly method, mixing the nano-encapsulated molecular sieve with a dry slice of a synthetic fiber, carrying out melt granulation and spinning to obtain a surface layer and a bottom layer, and encapsulating a filament raw material by using the molecular sieve; then uniformly mixing the nano-encapsulated composite wave-absorbing monofilament with conductive carbon black, drying the nano-encapsulated composite wave-absorbing monofilament with synthetic fiber slices, melting, granulating and spinning to obtain a nano-encapsulated composite wave-absorbing monofilament; then weaving the three-dimensional structure wave-absorbing textile by adopting a Raschel double-needle bed warp knitting machine, wherein the raw materials of the surface layer and the bottom layer are prepared molecular sieve packaging filaments; the spacing filament adopts a nano-encapsulated composite wave-absorbing monofilament; and finally, performing vacuum sputtering metal plating on the outside of the bottom layer of the three-dimensional structure wave-absorbing textile. The electromagnetic shielding material has good electromagnetic shielding efficiency, light weight, ventilation and good bearing function, and can be used for preventing electromagnetic interference in related fields.

Description

Preparation method of three-dimensional light-weight structural composite electromagnetic shielding material
Technical Field
The invention belongs to the technical field of preparation of electromagnetic shielding materials, and particularly relates to a preparation method of a three-dimensional light-weight structural type composite electromagnetic shielding material.
Background
The wave-absorbing material can effectively absorb incident electromagnetic waves and convert electromagnetic energy into heat energy to be dissipated, or the electromagnetic waves disappear through interference. With the rapid development of the electronics industry, the interference and pollution of electromagnetic waves become more serious. High-frequency communication, microwave heating, increasingly important radar stealth and electromagnetic compatibility (EMC) technologies and the like all need to adopt wave-absorbing materials to prevent electromagnetic radiation and leakage, protect the health and safety of human bodies, or achieve the purpose of radar stealth. The structural wave-absorbing material can bear and absorb waves, and is deeply valued by research personnel. At present, most structural wave-absorbing materials adopt different substrates for compounding, and some substrates are hollowed and filled with an absorbent or made into a honeycomb shape. The three-dimensional spacer fabric has a unique spacer structure, good air permeability, excellent supporting performance and the like, and the structure is effectively combined with the electromagnetic shielding function, so that the new application field of the wave-absorbing material can be widened. At present, the development and research of the wave-absorbing material by utilizing the three-dimensional space fabric are rare. Chinese patent (application number: 2017114392863, publication number: CN 108035049A) discloses an electromagnetic shielding fabric with a three-dimensional structure and a preparation method thereof, but the method only uses the three-dimensional fabric as a carrier, and an absorbent is filled in an interlayer of the three-dimensional fabric and is subjected to fluffing treatment, so that the prepared electromagnetic shielding fabric still belongs to a coating type wave-absorbing material, and the weight gain rate of the electromagnetic shielding fabric is still higher.
Disclosure of Invention
The invention aims to provide a preparation method of a three-dimensional light-weight structural composite electromagnetic shielding material, which has the advantages of light weight, ventilation and certain supporting function while ensuring the electromagnetic shielding function.
The technical scheme adopted by the invention is that the preparation method of the three-dimensional light structure type composite electromagnetic shielding material is implemented according to the following steps:
step 1, adding hydrophobic nano Fe 3 O 4 Carrying out hydrophilic modification on the powder;
step 2, preparing the nano-encapsulated molecular sieve by adopting a layer-by-layer assembly method;
step 3, mixing the dried nano-encapsulated molecular sieve with the dry slices of the synthetic fibers under high-speed stirring according to the mass ratio of 1: 4-9, uniformly mixing, and performing melt granulation to prepare the functional master batch; and (3) carrying out vacuum dehydration and drying treatment on the functional master batches and the slices of the synthetic fibers according to a mass ratio of 1: 4-9, carrying out melt spinning to prepare a molecular sieve packaging filament raw material for the surface layer and the bottom layer;
step 4, uniformly mixing the nano-encapsulated molecular sieve with conductive carbon black to obtain composite wave-absorbing powder, and after carrying out vacuum dehydration and drying treatment on the composite wave-absorbing powder and the synthetic fiber slices, carrying out vacuum dehydration and drying treatment on the composite wave-absorbing powder and the synthetic fiber slices according to the mass ratio of 1: 4-9, performing melt granulation to prepare the composite wave-absorbing functional master batch; after the composite wave-absorbing master batch and the slices of the synthetic fibers are subjected to vacuum dehydration and drying treatment, the composite wave-absorbing master batch and the slices of the synthetic fibers are prepared by the following steps in a mass ratio of 1: 4-9, performing melt spinning to prepare a nano-encapsulated composite wave-absorbing monofilament raw material for the core layer;
step 5, weaving the three-dimensional structure wave-absorbing textile by adopting a Raschel double-needle bed warp knitting machine, wherein the surface layer and the bottom layer of the textile are warp flat tissues with compact structures, and the surface layer and the bottom layer are the molecular sieve packaging filaments prepared in the step 3; the spacing filament adopts the nano-encapsulated composite wave-absorbing monofilament prepared in the step 4;
and 6, performing vacuum sputtering of a metal coating on the outside of the bottom layer of the three-dimensional structure wave-absorbing textile prepared in the step 5 in a vacuum spraying mode to obtain the three-dimensional light-weight structure type electromagnetic shielding material.
The present invention is also characterized in that,
in the step 1, the method specifically comprises the following steps:
step 1.1, adding hydrophobic nano Fe 3 O 4 Ultrasonically dispersing the powder in n-hexane to obtain Fe 3 O 4 N-hexane mixed liquor A;
hydrophobic nano Fe 3 O 4 The particle size of the powder is 20-40 nm; the specific addition amount is Fe 3 O 4 Powder 50g, n-hexane 10L; the ultrasonic dispersion time is 30min;
step 1.2, adding polyacrylic acid into DMF, and carrying out ultrasonic oscillation for 20-30 min to blend the polyacrylic acid and the DMF to obtain polyacrylic acid/DMF blended solution B;
the specific adding amount is 50ml of polyacrylic acid, and the adding amount of DMF is 5000ml;
step 1.3, fe prepared in step 1.1 3 O 4 Adding the n-hexane mixed solution A into the polyacrylic acid/DMF blended solution B obtained in the step 1.2, carrying out ultrasonic layering treatment, and obtaining the hydrophilic polymer by adopting magnetic adsorptionWater modified Fe 3 O 4 And modified Fe 3 O 4 Pouring into 5000ml deionized water, adding 50g trisodium citrate, and performing ultrasonic treatment for 2h to enable Fe 3 O 4 Fully dispersing, then centrifugally cleaning for three times, finally ultrasonically dispersing the Fe into an absolute ethyl alcohol solution for 30min to obtain modified Fe 3 O 4 And (4) magnetic fluid.
In the step 2, the method specifically comprises the following steps:
step 2.1, dissolving 100g of NaOH in 1KG distilled water, and then adding 284.2g of silicon source to obtain mother liquor A;
step 2.2, dissolving 100g of NaOH in 1KG distilled water, and then adding 163.9g of sodium metaaluminate to obtain mother liquor B;
step 2.3, slowly adding the mother liquor A into the modified Fe at the temperature of 30 ℃ under the condition of fully stirring 3 O 4 And (2) dropwise adding the mother liquor B into the magnetic fluid under a mechanical stirring state, continuously mechanically stirring for 2.5 hours after forming gel, setting the rotation speed at 500 r/min, aging for 2-4 hours at 30 ℃, crystallizing for 6-10 hours at 90-100 ℃, pouring the prepared molecular sieve into a centrifuge tube, centrifugally cleaning for three times by using deionized water in a high-speed centrifuge, and drying for 4 hours to obtain the nano-encapsulated molecular sieve.
Step 3, after the nano-encapsulated molecular sieve, the synthetic fiber slices and the functional master batches are subjected to vacuum dehydration and drying treatment, the water content of the nano-encapsulated molecular sieve, the synthetic fiber slices and the functional master batches is required to be lower than 200ppm;
the high-speed stirring speed range is 400-600 r/min;
in step 4, after the composite wave-absorbing powder, the synthetic fiber slices and the composite wave-absorbing master batches are subjected to vacuum dehydration and drying treatment, the water content of the composite wave-absorbing powder, the synthetic fiber slices and the composite wave-absorbing master batches is required to be lower than 200ppm;
the diameter of the nano packaging wave-absorbing monofilament is 0.10 mm-0.24 mm; the synthetic fiber is one of terylene, chinlon or polypropylene.
The linear density of the filament raw materials packaged by the molecular sieves for the surface layer and the bottom layer is 44 dtex-110 dtex; the synthetic fiber is one of terylene, chinlon or polypropylene.
In step 4, the grade of the conductive carbon black is environment-friendly Super P, and the ash content is 0.01 percentSpecific surface area of 62m 2 (ii)/g, particle size 40nm; the mass ratio of the nano-encapsulated molecular sieve to the conductive carbon black is 1:0.5 to 1.
In the step 5, the yarn laying mode is preferably V-shaped or X-shaped, and the back of a filament spacing needle transversely moves 1-5 needles; the needle bed interval distance of the Raschel double needle bed warp knitting machine is 3 mm-20 mm.
In step 6, the plated metal is silver or copper, and the thickness of the plated metal layer is 10-30 μm.
The invention has the advantages of utilizing the pore structure of the molecular sieve, the molecular sieve and Fe 3 O 4 The coating structure can realize impedance matching between the material and a free space in a high frequency range (8-18 GHz), ensures low reflection of electromagnetic waves on the surface of the material, and simultaneously enables incident electromagnetic waves to be more effectively attenuated through the synergistic action of multiple loss mechanisms such as dielectric loss, magnetic loss, nano effect, bottom metal layer reflection loss and the like. The electromagnetic shielding material has good electromagnetic shielding efficiency, light weight, ventilation and good bearing function, and can be used for preventing electromagnetic interference in related fields.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention relates to a preparation method of a three-dimensional light-weight structural composite electromagnetic shielding material, which is implemented according to the following steps:
step 1, adding hydrophobic nano Fe 3 O 4 Carrying out hydrophilic modification on the powder, which specifically comprises the following steps:
step 1.1, adding hydrophobic nano Fe 3 O 4 Ultrasonically dispersing the powder in normal hexane to obtain Fe 3 O 4 N-hexane mixed liquor A;
hydrophobic nano Fe 3 O 4 The particle size of the powder is 20-40 nm; the specific addition amount is Fe 3 O 4 Powder 50g, n-hexane 10L;
the ultrasonic dispersion time is 30min;
step 1.2, adding polyacrylic acid into DMF, and carrying out ultrasonic oscillation for 20-30 min to blend the polyacrylic acid and the DMF to obtain polyacrylic acid/DMF blended solution B;
the specific adding amount is 50ml of polyacrylic acid, and the adding amount of DMF is 5000ml;
step 1.3, fe prepared in step 1.1 3 O 4 Adding the normal hexane mixed solution A into the polyacrylic acid/DMF mixed solution B obtained in the step 1.2, carrying out ultrasonic layering treatment, and obtaining the hydrophilically modified Fe by adopting magnetic adsorption 3 O 4 And modified Fe 3 O 4 Pouring into 5000ml deionized water, adding 50g trisodium citrate, and performing ultrasonic treatment for 2h to obtain Fe 3 O 4 Fully dispersing, then centrifugally cleaning for three times, finally ultrasonically dispersing the Fe into an absolute ethyl alcohol solution for 30min to obtain modified Fe 3 O 4 A magnetic fluid;
step 2, preparing the nano-encapsulated molecular sieve by adopting a layer-by-layer assembly method, which specifically comprises the following steps:
step 2.1, dissolving NaOH in distilled water, and then adding a silicon source to obtain a mother liquor A;
the specific addition amount is 100g of NaOH and 1KG of distilled water;
the silicon source is sodium silicate, and the adding amount is 284.2g;
step 2.2, dissolving NaOH in distilled water, and then adding an aluminum source to obtain a mother liquor B, wherein the aluminum source is sodium metaaluminate;
the specific addition amount is 100g of NaOH and 1KG of distilled water;
the aluminum source is sodium metaaluminate, and the adding amount is 163.9g;
step 2.3, slowly adding the mother liquor A into the modified Fe at the temperature of 30 ℃ under the condition of fully stirring 3 O 4 And (3) dropwise adding the mother liquor B into the magnetic fluid under a mechanical stirring state, and continuing to mechanically stir for 2.5 hours after gel is formed, wherein the set rotating speed is 500 revolutions per minute. And aging for 2-4 h at 30 ℃, and crystallizing for 6-10 h at 90-100 ℃. And pouring the prepared molecular sieve into a centrifuge tube, centrifugally cleaning the molecular sieve in a high-speed centrifuge by using deionized water for three times, and drying the molecular sieve for 4 hours to obtain the nano-encapsulated molecular sieve.
Step 3, mixing the vacuum-dried nano-encapsulated molecular sieve with the dry slices of the synthetic fibers under the high-speed stirring of 400-600 revolutions per minute in a mass ratio of 1: 4-9, uniformly mixing, and performing melt granulation to prepare the functional master batch; and (3) carrying out vacuum dehydration and drying treatment on the functional master batches and the slices of the synthetic fibers according to the mass ratio of 1: 4-9, performing melt spinning to prepare a surface layer and a bottom layer of the three-dimensional light composite electromagnetic shielding material, and packaging filament raw materials by using a molecular sieve; the linear density of the filament molecular sieve packaging raw materials for the surface layer and the bottom layer is 44 dtex-110 dtex;
the synthetic fiber is any one of terylene, chinlon and polypropylene;
vacuum dehydrating and drying the raw materials by a vacuum dryer, wherein the vacuum degree is 95KPa, and the drying time is 10h; the water content of the dried nano packaging molecular sieve, the dried functional master batch and the dried synthetic fiber slice is less than 200ppm.
Step 4, uniformly mixing the nano-encapsulated molecular sieve with conductive carbon black to obtain composite wave-absorbing powder, and performing vacuum dehydration and drying treatment on the composite wave-absorbing powder and the slices of the synthetic fibers according to the mass ratio of the composite wave-absorbing powder to the slices of 1: 4-9, performing melt granulation to prepare the composite wave-absorbing functional master batch; and (2) carrying out vacuum dehydration and drying treatment on the composite wave-absorbing master batch and the slices of the synthetic fiber, wherein the mass ratio of the composite wave-absorbing master batch to the slices of the synthetic fiber is 1: 4-9, performing melt spinning to prepare a nano-encapsulated composite wave-absorbing monofilament raw material for the core layer; the diameter of the nano packaging composite wave-absorbing monofilament is 0.10 mm-0.24 mm;
the particle diameter of the conductive carbon black is 40nm, the grade is environment-friendly Super P, the ash content is 0.01 percent, and the specific surface area is 62m 2 /g；
The mass ratio of the nano-encapsulated molecular sieve to the conductive carbon black is 1:0.5 to 1;
vacuum dehydrating and drying by a vacuum dryer at the vacuum degree speed of 95KPa for 10h; the water content of the dried composite wave-absorbing powder, the dried composite wave-absorbing master batch and the dried synthetic fiber slice is required to be lower than 200ppm;
the synthetic fiber is any one of terylene, chinlon and polypropylene;
step 5, weaving the three-dimensional structure wave-absorbing textile by using a Raschel double-needle bed warp knitting machine, wherein the surface layer and the bottom layer fabric tissue are warp flat tissues with compact structures, and the surface layer and the bottom layer raw materials are the molecular sieve packaging filaments prepared in the step 3; the spacing filament adopts the nano-encapsulated composite wave-absorbing monofilament prepared in the step 4, the yarn laying mode is V-shaped or X-shaped, and the needle back of the spacing filament transversely moves 1-5 needles; the needle bed interval distance of the Raschel double needle bed warp knitting machine is 3 mm-20 mm;
step 6, performing vacuum sputtering of a metal coating on the outside of the bottom layer of the three-dimensional structure wave-absorbing textile prepared in the step 5 in a vacuum spraying mode to obtain a three-dimensional light-weight structure type electromagnetic shielding material;
the plated metal is silver or copper, and the thickness of the plated metal layer is 10-30 μm.
The three-dimensional light structural electromagnetic shielding material prepared by the invention is composed of a wave-transmitting layer, an absorption layer and a reflection layer; the prepared composite electromagnetic shielding material ensures that electromagnetic waves are incident from a wave-transmitting layer with matched surface wave impedance through special structure and process design, enter a composite wave-absorbing interval absorption layer to perform synergistic action of multiple loss mechanisms of dielectric loss, magnetic loss, nanometer effect and the like of the electromagnetic waves, and residual electromagnetic waves are reflected by a metal layer at a bottom layer to enter the composite wave-absorbing interval absorption layer again, so that the electromagnetic shielding material realizes good electromagnetic shielding efficiency through multiple effective absorption, reflection and reabsorption, is light in weight and has unique functions of interval fabrics.
Example 1
The invention relates to a preparation method of a three-dimensional light-weight structural composite electromagnetic shielding material, which is implemented according to the following steps:
step 1, adding hydrophobic nano Fe 3 O 4 Carrying out hydrophilic modification on the powder, specifically:
step 1.1, adding hydrophobic nano Fe 3 O 4 Ultrasonically dispersing the powder in n-hexane to obtain Fe 3 O 4 N-hexane mixed liquor A;
hydrophobic nano Fe 3 O 4 The particle size of the powder is 20nm; the specific addition amount is Fe 3 O 4 Powder 50g, n-hexane 10L;
the ultrasonic dispersion time is 30min;
step 1.2, adding polyacrylic acid into DMF, and carrying out ultrasonic oscillation for 20min to blend the polyacrylic acid and the DMF to obtain polyacrylic acid/DMF blending solution B;
the volume ratio of polyacrylic acid to DMF is 1:10; the specific addition amount is 50ml of polyacrylic acid, and 5000ml of DMF;
step 1.3, fe prepared in step 1.1 3 O 4 Adding the n-hexane mixed solution A into the polyacrylic acid/DMF blended solution B obtained in the step 1.2, carrying out ultrasonic layering treatment, and obtaining the hydrophilic modified Fe by adopting magnetic adsorption 3 O 4 And modified Fe 3 O 4 Pouring into 5000ml deionized water, adding 50g trisodium citrate, and performing ultrasonic treatment for 2h to enable Fe 3 O 4 Fully dispersing, then centrifugally cleaning for three times, finally ultrasonically dispersing the Fe into an absolute ethyl alcohol solution for 30min to obtain modified Fe 3 O 4 A magnetic fluid;
step 2, preparing the nano-encapsulated molecular sieve by adopting a layer-by-layer assembly method, which specifically comprises the following steps:
step 2.1, dissolving NaOH in distilled water, and then adding a silicon source to obtain a mother liquor A;
the specific addition amount is 100g of NaOH and 1KG of distilled water;
the silicon source is sodium silicate, and the adding amount is 284.2g;
step 2.2, dissolving NaOH in distilled water, and then adding an aluminum source to obtain a mother liquor B;
the specific addition amount is 100g of NaOH and 1KG of distilled water;
the aluminum source is sodium metaaluminate, and the adding amount is 163.9g;
step 2.3, slowly adding the mother liquor A into the modified Fe at the temperature of 30 ℃ under the condition of fully stirring 3 O 4 And (3) dropwise adding the mother liquor B into the magnetic fluid under a mechanical stirring state, and continuing to mechanically stir for 2.5 hours after gel is formed, wherein the set rotating speed is 500 revolutions per minute. And aging at 30 deg.C for 2h, and crystallizing at 90 deg.C for 10h. And pouring the prepared molecular sieve into a centrifuge tube, centrifugally cleaning the molecular sieve for three times by using deionized water in a high-speed centrifuge, and drying the molecular sieve for 4 hours to obtain the nano-encapsulated molecular sieve.
Step 3, mixing the vacuum-dried nano-encapsulated molecular sieve with the polyester dried slices under the high-speed stirring of 400 revolutions per minute in a mass ratio of 1:4, uniformly mixing, and performing melt granulation to prepare the terylene functional master batch; and then, carrying out vacuum dehydration and drying treatment on the polyester functional master batch and the polyester slices according to the mass ratio of 1:4, carrying out melt spinning to prepare a surface layer and a bottom layer of the three-dimensional light composite electromagnetic shielding material, and packaging polyester filament yarn raw materials by using a molecular sieve; the linear density of the polyester filament yarn raw materials packaged by the molecular sieves for the surface layer and the bottom layer is 44dtex/24f;
vacuum dehydrating and drying the raw materials by using a vacuum dryer at the vacuum speed of 95KPa for 10h, wherein the water contents of the dried nano packaging molecular sieve, the dried terylene functional master batch and the dried terylene slices are respectively 190ppm, 180ppm and 195ppm;
step 4, mixing the nano-encapsulated molecular sieve prepared in the step 2 with conductive carbon black according to a mass ratio of 1:0.5, uniformly mixing to obtain composite wave-absorbing powder, and after carrying out vacuum dehydration drying treatment on the composite wave-absorbing powder and the polyester slices, carrying out vacuum dehydration drying treatment on the composite wave-absorbing powder and the polyester slices according to the mass ratio of the composite wave-absorbing powder to the polyester slices of 1:4, performing melt granulation to prepare the composite wave-absorbing terylene functional master batch; after the composite wave-absorbing polyester functional master batch and the polyester chips are subjected to vacuum dehydration and drying treatment, the two are mixed according to the mass ratio of 1:4, carrying out melt spinning to prepare a nano-packaging composite wave-absorbing polyester monofilament raw material used for the core layer; the diameter of the nano packaging composite wave-absorbing polyester monofilament is 0.10mm;
the particle diameter of the conductive carbon black is 40nm, the grade is environment-friendly Super P, the ash content is 0.01 percent, and the specific surface area is 62m 2 /g；
And (3) performing vacuum dehydration drying on the raw materials by using a vacuum dryer, wherein the vacuum speed is 95KPa, the drying time is 10h, and the water content of the dried composite wave-absorbing powder, the dried composite wave-absorbing terylene functional master batch and the dried terylene slices is 175ppm, 188ppm and 195ppm respectively.
Step 5, weaving the three-dimensional structure wave-absorbing textile by using a Raschel double-needle bed warp knitting machine, wherein the surface layer and the bottom layer of the textile are warp flat tissues with compact structures, and the surface layer and the bottom layer are the molecular sieve packaging polyester filament prepared in the step 3; the spacer filaments adopt the nano-encapsulated composite wave-absorbing polyester monofilaments prepared in the step 4, the yarn laying mode is X-shaped, and the needle backs of the spacer filaments transversely move 1 needle; the needle bed spacing distance of the Raschel double needle bed warp knitting machine is 3mm;
and 6, performing vacuum sputtering on a metal silver layer outside the bottom layer of the three-dimensional structure wave-absorbing textile prepared in the step 5 in a vacuum spraying mode, wherein the thickness of the plated metal silver is 10 mu m, and thus the three-dimensional light-weight structure type electromagnetic shielding material can be obtained.
Tests prove that the three-dimensional light composite electromagnetic shielding material prepared by the embodiment has three strong absorption peaks in the frequency domain of 8.0-18.0 GHz, and the absorption shielding efficiency of the three-dimensional light composite electromagnetic shielding material on electromagnetic waves at 8.9GHz reaches 15dB; the absorption shielding efficiency of the electromagnetic wave at 13.7GHz reaches 10dB; the absorption shielding efficiency of the electromagnetic wave at 17.0GHz reaches 20dB; the square meter gram weight of the material is 312g/m 2 Air permeability of 3570L/m 2 ·s。
Example 2
The invention relates to a preparation method of a three-dimensional light-weight structural composite electromagnetic shielding material, which is implemented according to the following steps:
step 1, adding hydrophobic nano Fe 3 O 4 Carrying out hydrophilic modification on the powder, specifically:
step 1.1, adding hydrophobic nano Fe 3 O 4 Ultrasonically dispersing the powder in n-hexane to obtain Fe 3 O 4 N-hexane mixed liquor A;
hydrophobic nano Fe 3 O 4 The particle size of the powder is 40nm; the specific addition amount is Fe 3 O 4 Powder 50g, n-hexane 10L;
the ultrasonic dispersion time is 30min;
step 1.2, adding polyacrylic acid into DMF, and carrying out ultrasonic oscillation for 30min to blend the polyacrylic acid and the DMF to obtain polyacrylic acid/DMF blending solution B;
the volume ratio of polyacrylic acid to DMF is 1:10; the specific adding amount is 50ml of polyacrylic acid, and the adding amount of DMF is 5000ml;
step 1.3, fe prepared in step 1.1 3 O 4 Adding the normal hexane mixed solution A into the polyacrylic acid/DMF mixed solution B obtained in the step 1.2, carrying out ultrasonic layering treatment, and obtaining the hydrophilically modified Fe by adopting magnetic adsorption 3 O 4 And modified Fe 3 O 4 Pouring into 5000ml for removingAdding 50g trisodium citrate into the seed water, and performing ultrasonic treatment for 2 hours to enable Fe 3 O 4 Fully dispersing, then centrifugally cleaning for three times, finally ultrasonically dispersing the Fe into an absolute ethyl alcohol solution for 30min to obtain modified Fe 3 O 4 A magnetic fluid;
step 2, preparing the nano-encapsulated molecular sieve by adopting a layer-by-layer assembly method, which specifically comprises the following steps:
step 2.1, dissolving NaOH in distilled water, and then adding a silicon source to obtain a mother liquor A;
the specific addition amount is 100g of NaOH and 1KG of distilled water;
the silicon source is sodium silicate, and the adding amount is 284.2g;
step 2.2, dissolving NaOH in distilled water, and then adding an aluminum source to obtain a mother liquor B;
the specific addition amount is 100g of NaOH and 1KG of distilled water;
the aluminum source is sodium metaaluminate, and the adding amount is 163.9g;
step 2.3, slowly adding the mother liquor A into the modified Fe at the temperature of 30 ℃ under the condition of fully stirring 3 O 4 And (3) dropwise adding the mother liquor B into the magnetic fluid under a mechanical stirring state, and continuing to mechanically stir for 2.5 hours after gel is formed, wherein the set rotating speed is 500 revolutions per minute. Aging at 30 deg.C for 4 hr, and crystallizing at 100 deg.C for 6 hr. And pouring the prepared molecular sieve into a centrifuge tube, centrifugally cleaning the molecular sieve in a high-speed centrifuge by using deionized water for three times, and drying the molecular sieve for 4 hours to obtain the nano-encapsulated molecular sieve.
Step 3, mixing the vacuum-dried nano-encapsulated molecular sieve with the chinlon vacuum-dried slices under high-speed stirring at 600 revolutions per minute in a mass ratio of 1:9, uniformly mixing, and performing melt granulation to prepare polyamide functional master batches; and then, carrying out vacuum dehydration and drying treatment on the functional master batch and the chinlon slices, wherein the mass ratio is 1:9, carrying out melt spinning to prepare a surface layer and a bottom layer of the three-dimensional light composite electromagnetic shielding material, and packaging the nylon filament raw material by using a molecular sieve; the linear density of the nylon filament raw materials packaged by the molecular sieves for the surface layer and the bottom layer is 110dtex/24f;
and 4, performing vacuum dehydration drying on the raw materials by using a vacuum dryer, wherein the vacuum speed is 95KPa, the drying time is 10 hours, and the water contents of the dried nano packaging molecular sieve, the dried nylon chips and the dried nylon functional master batches are 190ppm, 190ppm and 182ppm respectively. Step 4, uniformly mixing the nano-encapsulated molecular sieve with conductive carbon black according to a mass ratio of 1:1 to obtain composite wave-absorbing powder, and after performing vacuum dehydration and drying treatment on the composite wave-absorbing powder and nylon chips, performing vacuum dehydration and drying treatment on the composite wave-absorbing powder and the nylon chips according to a mass ratio of 1:9, carrying out melt granulation to prepare the composite wave-absorbing polyamide functional master batch; after the composite wave-absorbing polyamide functional master batch and polyamide slices are subjected to vacuum dehydration and drying treatment, the two are mixed according to the mass ratio of 1:9, carrying out melt spinning to prepare a nano-packaging composite wave-absorbing polyamide monofilament raw material for the core layer; the diameter of the nano packaging composite wave-absorbing polyamide monofilament is 0.24mm;
the particle diameter of the conductive carbon black is 40nm, the grade is environment-friendly Super P, the ash content is 0.01 percent, and the specific surface area is 62m 2 /g；
And (3) performing vacuum dehydration drying on the raw materials by using a vacuum dryer, wherein the vacuum speed is 95KPa, the drying time is 10 hours, and the water contents of the dried composite wave-absorbing powder, the dried nylon slices and the dried composite wave-absorbing nylon functional master batches are 180ppm, 190ppm and 190ppm respectively.
Step 5, weaving the three-dimensional structure wave-absorbing textile by adopting a Raschel double-needle bed warp knitting machine, wherein the surface layer and the bottom layer of the textile are warp flat tissues with compact structures, and the surface layer and the bottom layer are prepared from the molecular sieve packaging nylon filament prepared in the step 3; the spacer wires adopt the nano-encapsulated composite wave-absorbing polyamide monofilaments prepared in the step 4, the yarn laying mode is V-shaped, and the needle backs of the spacer wires transversely move for 5 needles; the needle bed spacing distance of the Raschel double needle bed warp knitting machine is 20mm;
and 6, performing vacuum sputtering on a metal copper plating layer outside the bottom layer of the three-dimensional structure wave-absorbing textile prepared in the step 5 in a vacuum spraying mode, wherein the thickness of the plated metal copper is 30 mu m, and thus the three-dimensional light-weight structure type electromagnetic shielding material can be obtained.
Tests show that the three-dimensional light composite electromagnetic shielding material prepared by the embodiment has three strong absorption peaks in a frequency domain of 8.0-18.0 GHz, and the absorption shielding efficiency of the three-dimensional light composite electromagnetic shielding material on electromagnetic waves at 8.9GHz reaches 7dB; the absorption shielding efficiency of the electromagnetic wave at 13.7GHz reaches 5dB; absorption screen for electromagnetic wave at 17.0GHzThe shielding effect reaches 15dB; the square meter gram weight of the material is 1200g/m 2 The air permeability is 3190L/m 2 ·s。
Example 3
The invention relates to a preparation method of a three-dimensional light-weight structural composite electromagnetic shielding material, which is implemented according to the following steps:
step 1, adding hydrophobic nano Fe 3 O 4 Carrying out hydrophilic modification on the powder, which specifically comprises the following steps:
step 1.1, adding hydrophobic nano Fe 3 O 4 Ultrasonically dispersing the powder in n-hexane to obtain Fe 3 O 4 N-hexane mixed liquor A;
hydrophobic nano Fe 3 O 4 The particle size of the powder is 30nm; the specific addition amount is Fe 3 O 4 Powder 50g, n-hexane 10L;
the ultrasonic dispersion time is 30min;
step 1.2, adding polyacrylic acid into DMF, and carrying out ultrasonic oscillation for 25min to blend the polyacrylic acid and the DMF to obtain polyacrylic acid/DMF blended solution B;
the specific adding amount is 50ml of polyacrylic acid, and the adding amount of DMF is 5000ml;
step 1.3, fe prepared in step 1.1 3 O 4 Adding the n-hexane mixed solution A into the polyacrylic acid/DMF blended solution B obtained in the step 1.2, carrying out ultrasonic layering treatment, and obtaining the hydrophilic modified Fe by adopting magnetic adsorption 3 O 4 And modified Fe 3 O 4 Pouring into 5000ml deionized water, adding 50g trisodium citrate, and performing ultrasonic treatment for 2h to enable Fe 3 O 4 Fully dispersing, then centrifugally cleaning for three times, finally ultrasonically dispersing the Fe into an absolute ethyl alcohol solution for 30min to obtain modified Fe 3 O 4 A magnetic fluid;
step 2, preparing the nano-encapsulated molecular sieve by adopting a layer-by-layer assembly method, which specifically comprises the following steps:
step 2.1, dissolving NaOH in distilled water, and then adding a silicon source to obtain a mother liquor A;
the specific addition amount is 100g of NaOH and 1KG of distilled water;
the silicon source is sodium silicate, and the adding amount is 284.2g;
step 2.2, dissolving NaOH in distilled water, and then adding an aluminum source to obtain a mother liquor B;
the specific addition amount is 100g of NaOH and 1KG of distilled water;
the aluminum source is sodium metaaluminate, and the adding amount is 163.9g;
step 2.3, slowly adding the mother liquor A into the modified Fe at the temperature of 30 ℃ under the condition of fully stirring 3 O 4 And (3) dropwise adding the mother liquor B into the magnetic fluid under a mechanical stirring state, and continuing to mechanically stir for 2.5 hours after gel is formed, wherein the set rotating speed is 500 revolutions per minute. And aging at 30 deg.C for 2h, and crystallizing at 100 deg.C for 8h. And pouring the prepared molecular sieve into a centrifuge tube, centrifugally cleaning the molecular sieve in a high-speed centrifuge by using deionized water for three times, and drying the molecular sieve for 4 hours to obtain the nano-encapsulated molecular sieve.
And 3, stirring the vacuum-dried nano-encapsulation molecular sieve and the polyester dried slices at a high speed of 500 revolutions per minute in a mass ratio of 1:7, uniformly mixing, and carrying out melt granulation to prepare the functional master batch; and then, carrying out vacuum dehydration and drying treatment on the functional master batches and the slices of the synthetic fibers, wherein the mass ratio of the functional master batches to the slices of the synthetic fibers is 1:7, carrying out melt spinning to prepare a surface layer and a bottom layer of the three-dimensional light composite electromagnetic shielding material, and packaging polyester filament yarn raw materials by using a molecular sieve; the linear density of the polyester filament yarn raw materials packaged by the molecular sieves for the surface layer and the bottom layer is 78dtex/24f;
and (3) performing vacuum dehydration drying on the raw materials by using a vacuum dryer, wherein the vacuum speed is 95KPa, the drying time is 10h, and the water contents of the dried nano packaging molecular sieve, the dried terylene slices and the dried terylene functional master batches are 178ppm, 195ppm and 183ppm respectively.
Step 4, mixing the nano-encapsulated molecular sieve and the conductive carbon black according to a mass ratio of 1:0.75 uniform mixing to obtain composite wave-absorbing powder, and after carrying out vacuum dehydration drying treatment on the composite wave-absorbing powder and the polyester slices, the mass ratio of the composite wave-absorbing powder to the polyester slices is 1:7, performing melting granulation to prepare the composite wave-absorbing terylene functional master batch; carrying out vacuum dehydration and drying treatment on the composite wave-absorbing polyester functional master batch and polyester slices, and then mixing the master batch and the polyester slices according to the mass ratio of 1:7, carrying out melt spinning to prepare a nano-packaging composite wave-absorbing polyester monofilament raw material used for the core layer; the diameter of the nano packaging composite wave-absorbing polyester monofilament is 0.18mm;
the particle diameter of the conductive carbon black is 40nm, the grade is environment-friendly Super P, the ash content is 0.01 percent, and the specific surface area is 62m 2 /g；
And (3) performing vacuum dehydration drying on the raw materials by using a vacuum dryer, wherein the vacuum speed is 95KPa, the drying time is 10h, and the water content of the dried composite wave-absorbing powder, the dried terylene slices and the water content of the composite wave-absorbing terylene functional master batch are 168ppm, 195ppm and 177ppm respectively.
Step 5, weaving the three-dimensional structure wave-absorbing textile by using a Raschel double-needle bed warp knitting machine, wherein the surface layer and the bottom layer of the textile are warp flat tissues with compact structures, and the surface layer and the bottom layer are the molecular sieve packaging polyester filament prepared in the step 3; the spacer filaments adopt the nano-encapsulated composite wave-absorbing polyester monofilaments prepared in the step 4, the yarn laying mode is V-shaped, and the needle backs of the spacer filaments transversely move by 3 needles; the needle bed spacing distance of the Raschel double needle bed warp knitting machine is 12mm;
and 6, performing vacuum sputtering on a metal copper plating layer outside the bottom layer of the three-dimensional structure wave-absorbing textile prepared in the step 5 in a vacuum spraying mode, wherein the thickness of the plated metal copper is 20 mu m, and thus the three-dimensional light-weight structure type electromagnetic shielding material can be obtained.
Tests show that the three-dimensional light composite electromagnetic shielding material prepared by the embodiment has three strong absorption peaks in a frequency domain of 8.0-18.0 GHz, and the absorption shielding efficiency of the three-dimensional light composite electromagnetic shielding material on electromagnetic waves at 8.9GHz reaches 10.3dB; the absorption shielding efficiency of the electromagnetic wave at 13.7GHz reaches 7.5dB; the absorption shielding efficiency of 17.5dB on electromagnetic waves at 17.0GHz is achieved; the square meter gram weight of the material is 840g/m 2 The air permeability is 3310L/m 2 ·s。
Example 4
The invention relates to a preparation method of a three-dimensional light-weight structural composite electromagnetic shielding material, which is implemented according to the following steps:
step 1, adding hydrophobic nano Fe 3 O 4 Carrying out hydrophilic modification on the powder, specifically:
step 1.1, adding hydrophobic nano Fe 3 O 4 Ultrasonically dispersing the powder in n-hexane to obtainTo Fe 3 O 4 N-hexane mixed liquor A;
hydrophobic nano Fe 3 O 4 The particle size of the powder is 20nm; the specific addition amount is Fe 3 O 4 Powder 50g, n-hexane 10L;
the ultrasonic dispersion time is 30min;
step 1.2, adding polyacrylic acid into DMF, and carrying out ultrasonic oscillation for 20min to blend the polyacrylic acid and the DMF to obtain polyacrylic acid/DMF blending solution B;
the specific adding amount is 50ml of polyacrylic acid, and the adding amount of DMF is 5000ml;
step 1.3, fe prepared in step 1.1 3 O 4 Adding the n-hexane mixed solution A into the polyacrylic acid/DMF blended solution B obtained in the step 1.2, carrying out ultrasonic layering treatment, and obtaining the hydrophilic modified Fe by adopting magnetic adsorption 3 O 4 And modified Fe 3 O 4 Pouring into 5000ml deionized water, adding 50g trisodium citrate, and performing ultrasonic treatment for 2h to enable Fe 3 O 4 Fully dispersing, then centrifugally cleaning for three times, finally ultrasonically dispersing the Fe into an absolute ethyl alcohol solution for 30min to obtain modified Fe 3 O 4 A magnetic fluid;
step 2, preparing the nano-encapsulated molecular sieve by adopting a layer-by-layer assembly method, which specifically comprises the following steps:
step 2.1, dissolving NaOH in distilled water, and then adding a silicon source to obtain a mother liquor A;
the specific addition amount is 100g of NaOH and 1KG of distilled water;
the silicon source is sodium silicate, and the adding amount is 284.2g;
step 2.2, dissolving NaOH in distilled water, and then adding an aluminum source to obtain a mother liquor B;
the specific addition amount is 100g of NaOH and 1KG of distilled water;
the aluminum source is sodium metaaluminate, and the adding amount is 163.9g;
step 2.3, slowly adding the mother liquor A into the modified Fe at the temperature of 30 ℃ under the condition of fully stirring 3 O 4 Adding mother liquid B dropwise into the magnetic fluid under mechanical stirring to form gel, mechanically stirring for 2.5 hr, and rotatingThe speed is 500 revolutions per minute. Aging at 30 deg.C for 2.5h, and crystallizing at 90 deg.C for 9h. And pouring the prepared molecular sieve into a centrifuge tube, centrifugally cleaning the molecular sieve in a high-speed centrifuge by using deionized water for three times, and drying the molecular sieve for 4 hours to obtain the nano-encapsulated molecular sieve.
Step 3, mixing the vacuum-dried nano-encapsulated molecular sieve with the polypropylene dry slices under high-speed stirring at 450 revolutions per minute in a mass ratio of 1:5, uniformly mixing, and performing melt granulation to prepare polypropylene fiber functional master batch; after the polypropylene functional master batch and the polypropylene slices are subjected to vacuum dehydration and drying treatment, the weight ratio of the polypropylene functional master batch to the polypropylene slices is 1:5, carrying out melt spinning to prepare a surface layer and a bottom layer of the three-dimensional light composite electromagnetic shielding material, and packaging polypropylene filament raw materials by using a molecular sieve; the linear density of the polypropylene filament raw material packaged by the molecular sieve for the surface layer and the bottom layer is 60dtex/24f;
and (3) performing vacuum dehydration drying on the raw materials by using a vacuum dryer, wherein the vacuum speed is 95KPa, the drying time is 10h, and the water content of the dried nano packaging molecular sieve, the dried polypropylene slice and the dried polypropylene functional master batch is 185ppm, 190ppm and 180ppm respectively.
Step 4, mixing the nano-encapsulated molecular sieve and the conductive carbon black according to a mass ratio of 1:0.6 uniform mixing, obtain compound and inhale ripples powder, carry out vacuum dehydration drying process with compound ripples powder and polypropylene fibre section, according to compound ripples powder and the section mass ratio of inhaling 1:5, carrying out melt granulation to prepare the master batch with the composite wave-absorbing function; after the composite wave-absorbing master batch and the slices of the synthetic fibers are subjected to vacuum dehydration and drying treatment, the composite wave-absorbing master batch and the slices of the synthetic fibers are mixed according to the mass ratio of 1:5, carrying out melt spinning to prepare a nano-encapsulated composite wave-absorbing polypropylene fiber monofilament raw material used for the core layer; the diameter of the nano packaging composite wave-absorbing polypropylene fiber monofilament is 0.12mm;
the particle diameter of the conductive carbon black is 40nm, the grade is environment-friendly Super P, the ash content is 0.01 percent, and the specific surface area is 62m 2 /g；
And (3) performing vacuum dehydration drying on the raw materials by using a vacuum dryer, wherein the vacuum speed is 95KPa, the drying time is 10 hours, and the water contents of the dried composite wave-absorbing powder, the dried polypropylene slices and the dried composite wave-absorbing polypropylene functional master batches are 178ppm, 190ppm and 187ppm respectively.
Step 5, weaving the three-dimensional structure wave-absorbing textile by adopting a Raschel double-needle bed warp knitting machine, wherein the surface layer and the bottom layer of the textile are warp flat tissues with compact structures, and the surface layer and the bottom layer are prepared from the molecular sieve packaging polypropylene filament yarns prepared in the step 3; the spacing filament adopts the nano-encapsulated composite wave-absorbing polypropylene monofilament prepared in the step 4, the yarn laying mode is X-shaped, and the needle back of the spacing filament transversely moves 2 needles; the needle bed spacing distance of the Raschel double needle bed warp knitting machine is 6mm;
and 6, performing vacuum sputtering on a metal silver plating layer outside the bottom layer of the three-dimensional structure wave-absorbing textile prepared in the step 5 in a vacuum spraying mode to obtain the three-dimensional light-weight structure type electromagnetic shielding material, wherein the thickness of the plated metal silver is 15 mu m.
Tests show that the three-dimensional light composite electromagnetic shielding material prepared by the embodiment has three strong absorption peaks in the frequency domain of 8.0-18.0 GHz, and the absorption shielding efficiency of the three-dimensional light composite electromagnetic shielding material on electromagnetic waves at 8.9GHz reaches 12.3dB; the absorption shielding efficiency of the electromagnetic wave at 13.7GHz reaches 8.5dB; the absorption shielding effectiveness of the electromagnetic wave at 17.0GHz reaches 18.0dB; the square meter gram weight of the material is 460g/m 2 The air permeability is 3420L/m 2 ·s。
Example 5
The invention relates to a preparation method of a three-dimensional light-weight structural composite electromagnetic shielding material, which is implemented according to the following steps:
step 1, adding hydrophobic nano Fe 3 O 4 Carrying out hydrophilic modification on the powder, specifically:
step 1.1, adding hydrophobic nano Fe 3 O 4 Ultrasonically dispersing the powder in normal hexane to obtain Fe 3 O 4 N-hexane mixed liquor A;
hydrophobic nano Fe 3 O 4 The particle size of the powder is 40nm; the specific addition amount is Fe 3 O 4 Powder 50g, n-hexane 10L;
the ultrasonic dispersion time is 30min;
step 1.2, adding polyacrylic acid into DMF, and carrying out ultrasonic oscillation for 30min to blend the polyacrylic acid and the DMF to obtain polyacrylic acid/DMF blending solution B;
the specific addition amount is 50ml of polyacrylic acid, and 5000ml of DMF;
step 1.3, fe prepared in step 1.1 3 O 4 Adding the n-hexane mixed solution A into the polyacrylic acid/DMF blended solution B obtained in the step 1.2, carrying out ultrasonic layering treatment, and obtaining the hydrophilic modified Fe by adopting magnetic adsorption 3 O 4 And modified Fe 3 O 4 Pouring into 5000ml deionized water, adding 50g trisodium citrate, and performing ultrasonic treatment for 2h to enable Fe 3 O 4 Fully dispersing, then centrifugally cleaning for three times, finally ultrasonically dispersing the Fe into an absolute ethyl alcohol solution for 30min to obtain modified Fe 3 O 4 A magnetic fluid;
step 2, preparing the nano-encapsulated molecular sieve by adopting a layer-by-layer assembly method, which specifically comprises the following steps:
step 2.1, dissolving NaOH in distilled water, and then adding a silicon source to obtain a mother liquor A;
the specific addition amount is 100g of NaOH and 1KG of distilled water;
the silicon source is sodium silicate, and the adding amount is 284.2g;
step 2.2, dissolving NaOH in distilled water, and then adding an aluminum source to obtain a mother solution B; the specific addition amount is 100g of NaOH and 1KG of distilled water;
the aluminum source is sodium metaaluminate, and the adding amount is 163.9g;
step 2.3, slowly adding the mother liquor A into the modified Fe at the temperature of 30 ℃ under the condition of fully stirring 3 O 4 And (3) dropwise adding the mother liquor B into the magnetic fluid under a mechanical stirring state, and continuing to mechanically stir for 2.5 hours after gel is formed, wherein the set rotating speed is 500 revolutions per minute. Aging at 30 deg.C for 3.5h, and crystallizing at 95 deg.C for 7h. And pouring the prepared molecular sieve into a centrifuge tube, centrifugally cleaning the molecular sieve in a high-speed centrifuge by using deionized water for three times, and drying the molecular sieve for 4 hours to obtain the nano-encapsulated molecular sieve.
Step 3, mixing the vacuum-dried nano-encapsulated molecular sieve and the polypropylene dry slices under high-speed stirring at 600 revolutions per minute in a mass ratio of 1:8, uniformly mixing, and performing melt granulation to prepare polypropylene fiber functional master batch; and then, carrying out vacuum dehydration and drying treatment on the polypropylene functional master batch and the polypropylene slices in a mass ratio of 1:8, carrying out melt spinning to prepare a surface layer and a bottom layer of the three-dimensional light composite electromagnetic shielding material, and packaging polypropylene filament raw materials by using a molecular sieve; the linear density of the polypropylene filament raw material packaged by the molecular sieve for the surface layer and the bottom layer is 96dtex/24f;
vacuum dehydrating and drying the raw materials by using a vacuum dryer at the vacuum speed of 95KPa for 10h, wherein the water content of the dried nano packaging molecular sieve, the dried polypropylene slices and the dried polypropylene functional master batches is 190ppm, 190ppm and 185ppm respectively;
step 4, mixing the nano-encapsulated molecular sieve and the conductive carbon black according to a mass ratio of 1:0.9, obtaining composite wave-absorbing powder, carrying out vacuum dehydration and drying treatment on the composite wave-absorbing powder and the polypropylene slices, wherein the mass ratio of the composite wave-absorbing powder to the polypropylene slices is 1:8, performing melt granulation to prepare the composite wave-absorbing functional master batch; after the composite wave-absorbing master batch and the slices of the synthetic fibers are subjected to vacuum dehydration and drying treatment, the composite wave-absorbing master batch and the slices of the synthetic fibers are prepared by the following steps in a mass ratio of 1:8, carrying out melt spinning to prepare a nano-encapsulation wave-absorbing monofilament raw material used for the core layer; the diameter of the nano packaging wave-absorbing monofilament is 0.20mm;
the particle diameter of the conductive carbon black is 40nm, the grade is environment-friendly Super P, the ash content is 0.01 percent, and the specific surface area is 62m 2 /g；
And (3) performing vacuum dehydration drying on the raw materials by using a vacuum dryer, wherein the vacuum speed is 95KPa, the drying time is 10 hours, and the water contents of the dried composite wave-absorbing powder, the dried polypropylene slices and the dried composite wave-absorbing polypropylene functional master batches are 178ppm, 190ppm and 185ppm respectively.
Step 5, weaving the three-dimensional structure wave-absorbing textile by adopting a Raschel double-needle bed warp knitting machine, wherein the surface layer and the bottom layer of the textile are warp flat tissues with compact structures, and the surface layer and the bottom layer are prepared from the molecular sieve packaging polypropylene filament yarns prepared in the step 3; the spacing filament adopts the nano-encapsulated composite wave-absorbing polypropylene monofilament prepared in the step 4, the yarn laying mode is X-shaped, and the needle back of the spacing filament transversely moves 4 needles; the needle bed spacing distance of the Raschel double needle bed warp knitting machine is 18mm;
and 6, performing vacuum sputtering on a metal silver coating layer on the outer part of the bottom layer of the three-dimensional structure wave-absorbing textile prepared in the step 5 in a vacuum spraying mode to obtain the three-dimensional light-weight structure type electromagnetic shielding material, wherein the thickness of the metal silver coating is 25 micrometers.
Tests show that the three-dimensional light composite electromagnetic shielding material prepared by the embodiment has three strong absorption peaks in the frequency domain of 8.0-18.0 GHz, and the absorption shielding efficiency of the three-dimensional light composite electromagnetic shielding material on electromagnetic waves at 8.9GHz reaches 7.5dB; the absorption shielding efficiency of the electromagnetic wave at 13.7GHz reaches 6.8dB; the absorption shielding efficiency of the electromagnetic wave at 17.0GHz reaches 14.9dB; the square meter gram weight of the material is 1160g/m 2 The air permeability is 3150L/m 2 ·s。
Example 6
The invention relates to a preparation method of a three-dimensional light-weight structural composite electromagnetic shielding material, which is implemented according to the following steps:
step 1, adding hydrophobic nano Fe 3 O 4 Carrying out hydrophilic modification on the powder, specifically:
step 1.1, adding hydrophobic nano Fe 3 O 4 Ultrasonically dispersing the powder in normal hexane to obtain Fe 3 O 4 N-hexane mixed liquor A;
hydrophobic nano Fe 3 O 4 The particle size of the powder is 30nm; the specific addition amount is Fe 3 O 4 Powder 50g, n-hexane 10L;
the ultrasonic dispersion time is 30min;
step 1.2, adding polyacrylic acid into DMF, and carrying out ultrasonic oscillation for 30min to blend the polyacrylic acid and the DMF to obtain polyacrylic acid/DMF blending solution B;
the specific adding amount is 50ml of polyacrylic acid, and the adding amount of DMF is 5000ml;
step 1.3, fe prepared in step 1.1 3 O 4 Adding the normal hexane mixed solution A into the polyacrylic acid/DMF mixed solution B obtained in the step 1.2, carrying out ultrasonic layering treatment, and obtaining the hydrophilically modified Fe by adopting magnetic adsorption 3 O 4 And modified Fe 3 O 4 Pouring into 5000ml deionized water, adding 50g trisodium citrate, and performing ultrasonic treatment for 2h to enable Fe 3 O 4 Fully dispersing, then centrifugally cleaning for three times, finally ultrasonically dispersing the Fe into an absolute ethyl alcohol solution for 30min to obtain modified Fe 3 O 4 A magnetic fluid;
step 2, preparing the nano-encapsulated molecular sieve by adopting a layer-by-layer assembly method, which specifically comprises the following steps:
step 2.1, dissolving NaOH in distilled water, and then adding a silicon source to obtain a mother liquor A;
the specific addition amount is 100g of NaOH and 1KG of distilled water;
the silicon source is sodium silicate, and the adding amount is 284.2g;
step 2.2, dissolving NaOH in distilled water, and then adding an aluminum source to obtain a mother liquor B;
the specific addition amount is 100g of NaOH and 1KG of distilled water;
the aluminum source is sodium metaaluminate, and the adding amount is 163.9g;
step 2.3, slowly adding the mother liquor A into the modified Fe at the temperature of 30 ℃ under the condition of fully stirring 3 O 4 And (3) dropwise adding the mother liquor B into the magnetic fluid under a mechanical stirring state, and continuing to mechanically stir for 2.5 hours after gel is formed, wherein the set rotating speed is 500 revolutions per minute. Aging at 30 deg.C for 2.5h, and crystallizing at 100 deg.C for 6.5h. And pouring the prepared molecular sieve into a centrifuge tube, centrifugally cleaning the molecular sieve in a high-speed centrifuge by using deionized water for three times, and drying the molecular sieve for 4 hours to obtain the nano-encapsulated molecular sieve.
Step 3, mixing the vacuum-dried nano-encapsulated molecular sieve with the dried chinlon slices under high-speed stirring at 450 revolutions per minute in a mass ratio of 1:6, uniformly mixing, and performing melt granulation to prepare polyamide functional master batches; carrying out vacuum dehydration and drying treatment on the polyamide functional master batch and polyamide slices according to the mass ratio of 1:6, carrying out melt spinning to prepare a surface layer and a bottom layer of the three-dimensional light composite electromagnetic shielding material, and packaging the nylon filament raw material by using a molecular sieve; the linear density of the nylon filament raw materials packaged by the molecular sieves for the surface layer and the bottom layer is 100dtex/24f;
vacuum dehydrating and drying the raw materials by using a vacuum dryer at the vacuum speed of 95KPa for 10h, wherein the water contents of the dried nano packaging molecular sieve, the dried nylon slices and the dried nylon functional master batches are 165ppm, 190ppm and 175ppm respectively;
step 4, mixing the nano-encapsulated molecular sieve and the conductive carbon black according to a mass ratio of 1:0.8, obtaining composite wave-absorbing powder, and after carrying out vacuum dehydration and drying treatment on the composite wave-absorbing powder and the slices of the synthetic fibers, according to the mass ratio of the composite wave-absorbing powder to the slices of 1:6, carrying out melt granulation to prepare the master batch with the composite wave-absorbing function; and (2) carrying out vacuum dehydration and drying treatment on the composite wave-absorbing master batch and the slices of the synthetic fiber, and then mixing the master batch with the synthetic fiber according to the mass ratio of 1:6, carrying out melt spinning to prepare a nano-packaging composite wave-absorbing polyamide monofilament raw material used for the core layer; the diameter of the nano packaging composite wave-absorbing polyamide monofilament is 0.16mm;
the particle diameter of the conductive carbon black is 40nm, the grade is environment-friendly Super P, the ash content is 0.01 percent, and the specific surface area is 62m 2 /g；
And (3) performing vacuum dehydration drying on the raw materials by using a vacuum dryer, wherein the vacuum speed is 95KPa, the drying time is 10h, and the water contents of the dried composite wave-absorbing powder, the dried nylon slices and the composite wave-absorbing nylon functional master batches are 169ppm, 190ppm and 188ppm respectively.
Step 5, weaving the three-dimensional structure wave-absorbing textile by adopting a Raschel double-needle bed warp knitting machine, wherein the surface layer and the bottom layer of the textile are warp flat tissues with compact structures, and the surface layer and the bottom layer are prepared from the molecular sieve packaging nylon filament prepared in the step 3; the spacer wires adopt the nano-encapsulated composite wave-absorbing polyamide monofilaments prepared in the step 4, the yarn laying mode is V-shaped, and the needle backs of the spacer wires transversely move for 5 needles; the needle bed spacing distance of the Raschel double needle bed warp knitting machine is 15mm;
and 6, performing vacuum sputtering on a metal silver plating layer outside the bottom layer of the three-dimensional structure wave-absorbing textile prepared in the step 5 in a vacuum spraying mode to obtain the three-dimensional light-weight structure type electromagnetic shielding material, wherein the thickness of the plated metal silver is 28 micrometers.
Tests show that the three-dimensional light composite electromagnetic shielding material prepared by the embodiment has three strong absorption peaks in the frequency domain of 8.0-18.0 GHz, and the absorption shielding efficiency of the three-dimensional light composite electromagnetic shielding material on electromagnetic waves at 8.9GHz reaches 11.5dB; the absorption shielding efficiency of the electromagnetic wave at 13.7GHz reaches 7.9dB; the absorption shielding efficiency of the electromagnetic wave at 17.0GHz reaches 17.2dB; the gram weight of the material in square meter is 820g/m 2 Air permeability of 3270L/m 2 ·s。

Claims (7)

1. A preparation method of a three-dimensional light structure type composite electromagnetic shielding material is characterized by comprising the following steps:
step 1, adding hydrophobic nano Fe 3 O 4 Carrying out hydrophilic modification on the powder; the method specifically comprises the following steps:
step 1.1, adding hydrophobic nano Fe 3 O 4 Ultrasonically dispersing the powder in n-hexane to obtain Fe 3 O 4 N-hexane mixed liquor A;
hydrophobic nano Fe 3 O 4 The particle size of the powder is 20-40 nm; the specific addition amount is Fe 3 O 4 Powder 50g, n-hexane 10L; the ultrasonic dispersion time is 30min;
step 1.2, adding polyacrylic acid into DMF, and carrying out ultrasonic oscillation for 20-30 min to blend the polyacrylic acid and the DMF to obtain polyacrylic acid/DMF blended solution B;
the specific adding amount is 50ml of polyacrylic acid, and the adding amount of DMF is 5000ml;
step 1.3, fe prepared in step 1.1 3 O 4 Adding the normal hexane mixed solution A into the polyacrylic acid/DMF mixed solution B obtained in the step 1.2, carrying out ultrasonic layering treatment, and obtaining the hydrophilically modified Fe by adopting magnetic adsorption 3 O 4 And modified Fe 3 O 4 Pouring into 5000ml deionized water, adding 50g trisodium citrate, and performing ultrasonic treatment for 2h to obtain Fe 3 O 4 Fully dispersing, then centrifugally cleaning for three times, finally ultrasonically dispersing the Fe into an absolute ethyl alcohol solution for 30min to obtain modified Fe 3 O 4 A magnetic fluid;
step 2, preparing the nano-encapsulated molecular sieve by adopting a layer-by-layer assembly method;
step 3, mixing the dried nano-encapsulated molecular sieve with the dry slices of the synthetic fibers under high-speed stirring according to the mass ratio of 1: 4-9, uniformly mixing, and performing melt granulation to prepare the functional master batch; and (3) carrying out vacuum dehydration and drying treatment on the functional master batches and the slices of the synthetic fibers according to the mass ratio of 1: 4-9, carrying out melt spinning to prepare a molecular sieve packaging filament raw material for the surface layer and the bottom layer;
step 4, uniformly mixing the nano-encapsulated molecular sieve with conductive carbon black according to the mass ratio of 1.5-1 to obtain composite wave-absorbing powder, and after carrying out vacuum dehydration and drying treatment on the composite wave-absorbing powder and the slices of the synthetic fibers, then carrying out vacuum dehydration and drying treatment on the composite wave-absorbing powder and the slices of the synthetic fibers according to the mass ratio of 1: 4-9, performing melt granulation to prepare the composite wave-absorbing functional master batch; after the composite wave-absorbing master batch and the slices of the synthetic fibers are subjected to vacuum dehydration and drying treatment, the composite wave-absorbing master batch and the slices of the synthetic fibers are prepared by the following steps in a mass ratio of 1: 4-9, performing melt spinning to prepare a nano-encapsulated composite wave-absorbing monofilament raw material for the core layer;
step 5, weaving the three-dimensional structure wave-absorbing textile by adopting a Raschel double-needle bed warp knitting machine, wherein the surface layer and the bottom layer of the textile are warp flat tissues with compact structures, and the surface layer and the bottom layer are the molecular sieve packaging filaments prepared in the step 3; the spacing filament adopts the nano-encapsulated composite wave-absorbing monofilament prepared in the step 4;
and 6, performing vacuum sputtering of a metal coating on the outside of the bottom layer of the three-dimensional structure wave-absorbing textile prepared in the step 5 in a vacuum spraying mode to obtain the three-dimensional light-weight structure type electromagnetic shielding material.
2. The method for preparing a three-dimensional light structural type composite electromagnetic shielding material according to claim 1, wherein in the step 2, specifically:
step 2.1, dissolving 100g of NaOH in 1KG distilled water, and then adding 284.2g of silicon source to obtain mother liquor A;
step 2.2, dissolving 100g of NaOH in 1KG distilled water, and then adding 163.9g of sodium metaaluminate to obtain mother liquor B;
step 2.3, slowly adding the mother liquor A into the modified Fe at the temperature of 30 ℃ under the condition of fully stirring 3 O 4 And (2) dropwise adding the mother liquor B into the magnetic fluid under a mechanical stirring state, continuously mechanically stirring for 2.5 hours after gel is formed, setting the rotating speed at 500 r/min, aging for 2-4 hours at 30 ℃, crystallizing for 6-10 hours at 90-100 ℃, pouring the prepared molecular sieve into a centrifugal tube, centrifugally cleaning for three times by using deionized water in a high-speed centrifuge, and drying for 4 hours to obtain the nano-encapsulated molecular sieve.
3. The method for preparing a three-dimensional light structural type composite electromagnetic shielding material according to claim 1, wherein in the step 3, the linear density of the filament raw materials packaged by the molecular sieve for the surface layer and the bottom layer is 44 dtex-110 dtex; the synthetic fiber is any one of terylene, chinlon and polypropylene fiber.
4. The method for preparing a three-dimensional light structural type composite electromagnetic shielding material according to claim 1, wherein in the step 4, the diameter of the nano-encapsulated composite wave-absorbing monofilament is 0.10mm to 0.24mm; the synthetic fiber is any one of terylene, chinlon and polypropylene fiber.
5. The method for preparing a three-dimensional light structural type composite electromagnetic shielding material of claim 1, wherein in the step 4, the particle size of the conductive carbon black is 40nm.
6. The method for preparing a three-dimensional light structure type composite electromagnetic shielding material according to claim 1, wherein in the step 5, the yarn laying mode is V-shaped or X-shaped, and the back of a spacing filament needle transversely moves 1-5 needles; the needle bed interval distance of the Raschel double needle bed warp knitting machine is 3 mm-20 mm.
7. The method for preparing a three-dimensional light structural type composite electromagnetic shielding material according to claim 1, wherein in the step 6, the plated metal is silver or copper, and the thickness of the plated metal layer is 10-30 μm.
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KR100898587B1 (en) * 2008-08-25 2009-05-20 에스씨씨(주) Composition of non-woven fabric for shielding electro-magnetic wave
CN104841345A (en) * 2015-04-21 2015-08-19 西南交通大学 Photomagnetic dual-response Pickering emulsion coalescence reaction system and application thereof
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