CN110452464A - A kind of nano combined electromagnetic shielding material of resin base carbon and preparation method thereof - Google Patents

A kind of nano combined electromagnetic shielding material of resin base carbon and preparation method thereof Download PDF

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Publication number
CN110452464A
CN110452464A CN201910852594.1A CN201910852594A CN110452464A CN 110452464 A CN110452464 A CN 110452464A CN 201910852594 A CN201910852594 A CN 201910852594A CN 110452464 A CN110452464 A CN 110452464A
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electromagnetic shielding
shielding material
carbon nanotube
nano combined
resin base
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Inventor
李克训
马江将
张捷
贾琨
刘伟
谷建宇
马晨
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CETC 33 Research Institute
China Electronic Technology Cyber Security Co Ltd
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CETC 33 Research Institute
China Electronic Technology Cyber Security Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/002—Methods
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/02—Making granules by dividing preformed material
    • B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
    • B29C45/17—Component parts, details or accessories; Auxiliary operations
    • B29C45/76—Measuring, controlling or regulating
    • B29C45/78—Measuring, controlling or regulating of temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/92—Measuring, controlling or regulating
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/04—Homopolymers or copolymers of ethene
    • C08L23/06—Polyethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/10—Homopolymers or copolymers of propene
    • C08L23/12—Polypropene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L55/00—Compositions of homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C08L23/00 - C08L53/00
    • C08L55/02—ABS [Acrylonitrile-Butadiene-Styrene] polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2945/00—Indexing scheme relating to injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould
    • B29C2945/76—Measuring, controlling or regulating
    • B29C2945/76494—Controlled parameter
    • B29C2945/76531—Temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/9258—Velocity
    • B29C2948/9259—Angular velocity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92704—Temperature
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K2003/026—Phosphorus
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2217—Oxides; Hydroxides of metals of magnesium
    • C08K2003/2224—Magnesium hydroxide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/003—Additives being defined by their diameter
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
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    • C08K2201/004—Additives being defined by their length
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/02—Flame or fire retardant/resistant
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)

Abstract

The present invention relates to electromangnetic spectrum fields, more specifically, are related to a kind of nano combined electromagnetic shielding material of resin base carbon and preparation method thereof, and making carbon nanotube by synchronous addition fire retardant, plasticizer etc., it is well dispersed in thermoplastic resin matrix.The orthogonal array carbon nanotube that the present invention is obtained by chemical vapour deposition technique, to replace the metal fiber function additive in conventional resins base electromagnetic screen material, electromagnetic shielding material obtained is light, good dispersion, strong environmental adaptability, due to the high-specific surface area and nano effect of nano-carbon material, its additive amount is substantially reduced, and effectively prevent disorderly and unsystematic orientation carbon nanomaterial winding agglomerate caused by be difficult to the dispersion, and thereby result in resin matrix mechanical property reduce the problem of.The nano combined electromagnetic shielding material of resin base carbon of the present invention can be used for electronic information and household appliance technical field effectively to be shielded to electromagnetic radiation.

Description

A kind of nano combined electromagnetic shielding material of resin base carbon and preparation method thereof
Technical field
The present invention relates to electromangnetic spectrum fields, more specifically, are related to a kind of nano combined electromagnetic screen of resin base carbon Cover material and preparation method thereof.
Background technique
With the aggravation of current era IT application process, various electronic information equipments, all kinds of household electrical appliances are rapidly popularized；Automobile, The rapid development of the City Traffic Transport Systems such as electric car, subway, light rail and electric railway causes electromagnetic radiation to be in steeply rise Gesture.Electromagnetic pollution has become the fourth-largest pollution after water pollution, atmosphere pollution, noise pollution.Electromagnetic radiation not only can Electromagnetic interference and electromagnetic compatibility problem are brought, can also bring threat to the physical and mental health of the mankind.The work of electronic information instrument and equipment When the electromagnetic wave that gives off, the normal work of surrounding instruments equipment can be interfered, influence the decline of system performance, make to automatically control System down, Information Conduction fault etc., cause unpredictable catastrophic effect.Electromagnetic radiation to the vision of people, endocrine, Reproduction and heredity, body's immunity, central nervous system etc. have different degrees of influence, especially high frequency waves and relatively strong Electromagnetic field effect human body after, in the energy and strength dissolved for unconsciously leading to people, the biological clock of people is made to get muddled, Memory, thinking and judgement decline etc., or even cause certain lesions.All attach great importance to increasingly complicated electromagnetism ring in countries in the world It border and its is influenced caused by human lives, in order to protect environment, protection human health, ensure electronic information security, it is necessary to right Electromagnetic radiation is protected, and the protection of electromagnetic radiation pollution has been very urgent.
The polymer-based microwave defense material technical research that foreign countries carry out, is that surface conductance film is used for macromolecule material first Expect matrix, once but conductive film it is damaged, shield effectiveness is just affected；It is then multiple in processing of high molecular material forming process It closes into electroconductive stuffing, makes its processing and the primary completion of shielding, but influence factor is complex, including conductive filler itself and base Property, form, loading and degree of scatter of body material etc., it is closely related with the shield effectiveness of its polymer composite. Foreign countries are in such material product first based on thermoplastic resin matrix.Such as Japanese Zhong Fang company, Hitachi, Japan chemical conversion, U.S.'s cyanogen Amine company, Mitsubishi artificial silk etc., respectively to polycarbonate, ABS, nylon 6, polypropylene, polyvinyl chloride, polystyrene, The resin matrixes such as ABS, polypropylene have carried out conductive modified, and modifying agent is mainly Al, Fe fiber, stainless steel fibre, Cu fiber, plating Nickel graphite fibre, superfine carbon black etc. make it show certain shielding properties to electromagnetic radiation.But due to being with metallic fiber It is main, show the disadvantages of density is big, quality is heavy and easily corrodes.
Since carbon nanotube (CNTs) discovery, there is excellent intensity, hardness, bullet due to its special structure feature Property and the performances such as good calorifics and electricity, are widely used in preparing the function additive of high-performance composite materials.But longer In a period of time, since the mutual winding of CNTs keeps its dispersion problem in resin matrix prominent, and it is hindered multiple The performance of excellent properties when condensation material practical application.As scientific worker deepens continuously to CNTs research, orthogonal array carbon is received Prepared by mitron, be mainly used for the technical research such as electronic device and transparent conductive film preparation, meanwhile, compared to mutually winding Traditional preparation methods obtained CNTs, this CNTs obtained from orthogonal array showed in resin matrix by pre-processing Relatively excellent dispersion performance out.Therefore, the application with the CNTs of such special construction type be main function additive, to heat Plastic resin matrices are modified processing, it is made to have electro-magnetic screen function, to reduce the electromagnetic radiation pollution extent of injury.
Summary of the invention
In the presence of overcoming the shortcomings of the prior art, the present invention provides a kind of nano combined electromagnetic shielding of resin base carbon Material and preparation method thereof, solution carbon nanotube is evenly dispersed and its asks with electro-magnetic screen function enhancing of the resin matrix after compound Topic.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is as follows:
A kind of nano combined electromagnetic shielding material of resin base carbon, including thermoplastic resin and carbon nanotube, the carbon nanotube are adopted With vertical array column carbon nanotube；It disperses orthogonal array carbon nanotube in thermoplastic resin matrix, passes through mixed at high speed, note It moulds technique and electromagnetic shielding material is made.
A kind of preparation method of the nano combined electromagnetic shielding material of resin base carbon, comprising the following steps:
The preparation of S1, vertical array column carbon nanotube: utilizing chemical vapour deposition technique, and obtaining caliber is 10nm-20nm, and length is 10 μm -200 μm of vertical array column carbon nanotube；
S2, carbon nanotube preprocessing process: the vertical array column carbon nanotube prepared in S1 is peeled off from the substrate, and is weighed It is spare to measure plasticizer 10ml-100ml indwelling after preparatory mechanical stirring and ultrasonic disperse 20min-60min by 0.01g-1g；
S3, weighing: pressing mass fraction, weighs 100 parts of thermoplastic resin raw materials；Measure 5 parts of the plasticizer-for being mixed with carbon nanotube 20 parts；Weigh 1 part -3 parts of antioxidant；Measure 0.5 part -2 parts of silane coupling agent；Weigh 0.1 part -0.5 part of lubricant；Weigh hydrogen-oxygen Change one of aluminium, magnesium hydroxide and red phosphorus or totally 0.5 part -1.5 parts of a variety of mixing；Aluminium hydroxide, magnesium hydroxide and red phosphorus are made Cooperative flame retardant effect is played for fire retardant；
S4, it is stirred process: by thermoplastic resin raw materials as high-speed mixer, being arranged -80 DEG C of temperature 60 C, revolving speed 700r/min-1500r/min, time 10min-30min sequentially add coupling agent, the plasticizer, anti-dissolved with enough carbon nanotubes Oxygen agent, lubricant and fire retardant continue to stir 10min-30min；
S5, melting extrusion mixing: thermoplastic resin matrix and function additive through high-speed stirred mixing are placed in screw extruder, into Row melting mixing is granulated after squeezing out, and pellet partial size is 3mm-8mm, length 3mm-5mm；
S6, injection molding process: by pellet in S5 in 60 DEG C -85 DEG C dry 60min-120min, injection molding machine is added, finally obtains The nano combined electromagnetic shielding material of resin base carbon.
Further, the carbon nanotube chemical vapor deposition processes, using methane or ethylene as carbon-source gas, gas Flow is 100sccm-300sccm；Using argon gas as carrier gas, gas flow 200sccm ~ 250sccm；Using iron nano-film conduct Catalyst, film thickness 1nm-5nm；Reaction temperature is 600 DEG C -800 DEG C；Reaction time is 1min-30min.
Further, the plasticizer uses phthalic ester plasticizer；Or increased using phthalate Modeling agent is aided with fatty diacid ester plasticizer or epoxy ester series plasticizer mixed form.
Further, the phthalic ester plasticizer is that dioctyl phthalate or phthalic acid two are different pungent Ester；The fatty diacid ester plasticizer is dioctyl adipate；The epoxy ester series plasticizer is epoxidized soybean oil.
Further, the antioxidant includes tetrapentaerythritol ester, propionic acid octadecyl, 1,2 pairs of hydrazines.
Further, the lubricant is one of paraffin, chlorinated paraffin, calcium stearate.
Further, the thermoplastic resin raw materials are one of polypropylene, polyethylene, ABS plastic.
Further, when the thermoplastic resin raw materials are polypropylene or polyethylene, when melting mixing squeezes out, Screw Extrusion Machine temperature setting be 155 DEG C -165 DEG C, 165 DEG C -175 DEG C, 175 DEG C -185 DEG C, 185 DEG C -210 DEG C, 180 DEG C -195 DEG C of nozzle； The thermoplastic resin raw materials be ABS plastic when, melting mixing squeeze out when, screw extruder temperature setting be 160 DEG C -175 DEG C, 170 DEG C -185 DEG C, 180 DEG C -195 DEG C, 190 DEG C -210 DEG C, 185 DEG C -200 DEG C of nozzle；Screw extruder screw speed is 25r/ min-50r/min。
Further, the thermoplastic resin raw materials be polypropylene or polyethylene when, injection temperature be 160 DEG C -170 DEG C, 165 DEG C -180 DEG C, 170 DEG C -190 DEG C, 185 DEG C -205 DEG C, 180 DEG C -195 DEG C of spray head；The thermoplastic resin raw materials are ABS modeling When material, injection temperature be 165 DEG C -180 DEG C, 175 DEG C -190 DEG C, 185 DEG C -200 DEG C, 195 DEG C -220 DEG C, 190 DEG C -205 of spray head ℃。
Compared with prior art, the advantageous effect of present invention is that:
The present invention provides a kind of nano combined electromagnetic shielding materials of resin base carbon and preparation method thereof, fire-retardant by synchronous addition Agent, plasticizer etc. make carbon nanotube, and it is well dispersed in thermoplastic resin matrix.The present invention passes through chemical vapour deposition technique Obtained orthogonal array carbon nanotube, to replace the metal fiber function additive in conventional resins base electromagnetic screen material, system Electromagnetic shielding material is light, good dispersion, strong environmental adaptability, due to the high-specific surface area and nanometer of nano-carbon material Effect, additive amount are substantially reduced, and effectively prevent disorderly and unsystematic orientation carbon nanomaterial winding agglomerate caused by hardly possible With the dispersion, and thereby result in the problem of reducing to resin matrix mechanical property.The nano combined electricity of resin base carbon of the present invention Magnetic shielding material can be used for electronic information and household appliance technical field effectively to be shielded to electromagnetic radiation.
Detailed description of the invention
Fig. 1 is a kind of nano combined electromagnetic shielding material preparation flow figure of resin base carbon provided by the invention；
Fig. 2 is multi-walled carbon nanotube TEM figure；
Fig. 3 is that the multi-walled carbon nanotube SEM of specific length schemes；
Fig. 4 is the nano combined electromagnetic shielding material sample appearance figure of resin base carbon；
Fig. 5 is distribution figure of the carbon nanotube in resin matrix；
Fig. 6 is the nano combined electromagnetic shielding shielding properties of resin base carbon.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other Embodiment shall fall within the protection scope of the present invention.
A kind of nano combined electromagnetic shielding material of resin base carbon, including thermoplastic resin and carbon nanotube, the carbon nanometer Pipe uses vertical array column carbon nanotube；It disperses orthogonal array carbon nanotube in thermoplastic resin matrix, passes through high speed Electromagnetic shielding material is made in mixing, Shooting Technique.Preparation flow figure is as shown in Figure 1.
Embodiment one
A kind of preparation method of the nano combined electromagnetic shielding material of resin base carbon, comprising the following steps:
(1) preparation of specific structure carbon nanotube: utilizing chemical vapour deposition technique (CVD), using methane as carbon-source gas, gas stream Measure 150sccm-200sccm range, using argon gas as carrier gas, gas flow 200sccm-250sccm, reaction temperature 700 DEG C- Carbon nanotube is presented perpendicular to substrate in 750 DEG C, reaction time 5min-15min, catalyst Fe nano film thickness 2nm-3nm Array format growth, obtain caliber 10nm-20nm, 15 μm -50 μm of length of vertical array column carbon nanotube；
(2) carbon nanotube preprocessing process: previously prepared carbon nanotube in (1) is peeled off from the substrate, and weighs 0.01g- 0.5g is scattered in it in dioctyl phthalate (DOP) plasticizer by ultrasonic disperse instrument, measures plasticizer DOP 20ml-80ml, epoxidized soybean oil (ESO) assisted class plasticizer 10ml-30ml mixing, through preparatory mechanical stirring and ultrasonic disperse Indwelling is spare after 30min-50min；
(3) it weighs: pressing mass fraction, weigh 100 parts of PP resin raw material first；Measure 5 parts of the plasticizer-for being mixed with carbon nanotube 10 parts；1 part -1.5 parts of weighing tetrapentaerythritol ester (antioxidant 1010)；Measure 0.5 part -1.5 parts of silane coupling agent；Weigh chlorination 0.1 part -0.5 part of paraffin meter；Weigh 0.5 part -1.0 parts of aluminium hydroxide；
(4) it is stirred process: by PP as high-speed mixer, being arranged -80 DEG C of temperature 60 C, revolving speed 700r/min-1000r/ Min, time 10min-30min sequentially add coupling agent, the plasticizer dissolved with enough carbon nanotubes, antioxidant, lubricant and resistance The functional aids such as agent are fired, continue to stir 10min-30min；
(5) melting extrusion mixes: thermoplastic resin matrix and function additive through high-speed stirred mixing are placed in screw extruder, into Row melting mixing is respectively set temperature (four sections): 155 DEG C -165 DEG C, 165 DEG C -175 DEG C, 175 DEG C -185 DEG C, 185 DEG C -210 DEG C, 180 DEG C -195 DEG C of nozzle, screw speed 25r/min-50r/min, then extruding pelletization is cooling, and pellet partial size is 3mm- 8mm, length 3mm-5mm, for use；
(6) injection molding process: by the pellet after melting mixing in 60 DEG C -85 DEG C dry 60min-120min, being added injection molding machine, Temperature is arranged: 160 DEG C -170 DEG C, 165 DEG C -180 DEG C, 170 DEG C -190 DEG C, 185 DEG C -205 DEG C, will melt by 180 DEG C -195 DEG C of spray head Melt resin Material injection enters in preheated mold；Finally obtain the nano combined electromagnetic shielding material of resin base carbon.
Embodiment two
A kind of preparation method of the nano combined electromagnetic shielding material of resin base carbon, comprising the following steps:
(1) preparation of specific structure carbon nanotube: utilizing chemical vapour deposition technique (CVD), using ethylene as carbon-source gas, gas stream Measure 200sccm-250sccm range；Using argon gas as carrier gas, gas flow 250sccm-300sccm, reaction temperature 700 DEG C- Carbon nanotube is presented perpendicular to base in 750 DEG C, reaction time 15min-25min, catalyst Fe nano film thickness 2nm-3nm The array format at bottom is grown, and obtaining caliber is 10nm-20nm, the vertical array column carbon nanotube that length is 50 μm -100 μm；
(2) carbon nanotube preprocessing process: previously prepared carbon nanotube in (1) is peeled off from the substrate, and weighs 0.01g- 0.5g is scattered in it in dioctyl phthalate (DOP) plasticizer by ultrasonic disperse instrument, measures plasticizer DOP 20ml-80ml, dioctyl adipate (DOA) assisted class plasticizer 20ml-30ml mixing, through preparatory mechanical stirring and ultrasonic disperse Indwelling is spare after 30min-50min；
(3) it weighs: pressing mass fraction, weigh 100 parts of PP resin raw material first；Measure the plasticizer 10 for being mixed with carbon nanotube - 20 parts of part；Weigh 0.5 part -1.5 parts of tetrapentaerythritol ester (antioxidant 1010), propionic acid octadecyl (antioxidant 1076) 0.5 - 1.5 parts of part；Measure 1 part -2 parts of silane coupling agent；Weigh paraffin wax 0.1-0.3 parts, 0.1 part -0.2 part of calcium stearate；Claim Measure 0.5 part -1.0 parts of aluminium hydroxide, 0.1 part -0.5 part of red phosphorus；
(4) it is stirred process: PP being placed in high-speed mixer, is arranged -80 DEG C of temperature 60 C, revolving speed 1000r/min-1500r/ Min, time 10min-30min sequentially add coupling agent, the plasticizer dissolved with enough carbon nanotubes, antioxidant, lubricant and resistance The functional aids such as agent are fired, continue to stir 10min-30min；
(5) melting extrusion mixes: thermoplastic resin matrix and function additive through high-speed stirred mixing are placed in screw extruder, into Row melting mixing is respectively set temperature (four sections): 155 DEG C -165 DEG C, 165 DEG C -175 DEG C, 175 DEG C -185 DEG C, 185 DEG C -210 DEG C, 180 DEG C -195 DEG C of nozzle, screw speed 25r/min-50r/min, then extruding pelletization is cooling, pellet partial size 3mm-8mm, Length 3mm-5mm, for use；
(6) injection molding process: by the pellet after melting mixing in 60 DEG C -85 DEG C dry 60min-120min, being added injection molding machine, Temperature is arranged: 160 DEG C -170 DEG C, 165 DEG C -180 DEG C, 170 DEG C -190 DEG C, 185 DEG C -205 DEG C, will melt by 180 DEG C -195 DEG C of spray head Melt resin Material injection enters in preheated mold；Finally obtain the nano combined electromagnetic shielding material of resin base carbon.
Embodiment three
A kind of preparation method of the nano combined electromagnetic shielding material of resin base carbon, comprising the following steps:
(1) preparation of specific structure carbon nanotube: utilizing chemical vapour deposition technique (CVD), using ethylene as carbon-source gas, gas stream Measure 150sccm-200sccm range；Using argon gas as carrier gas, gas flow 200sccm-250sccm, reaction temperature 700 DEG C- Carbon nanotube is presented perpendicular to substrate in 750 DEG C, reaction time 5min-15min, catalyst Fe nano film thickness 2nm-3nm Array format growth, obtaining caliber is 10nm-20nm, and length is 15 μm -50 μm of vertical array column carbon nanotube；
(2) carbon nanotube preprocessing process: previously prepared carbon nanotube in (1) is peeled off from the substrate, and weighs 0.01g- 0.5g is scattered in it in dioctyl phthalate (DOP) plasticizer by ultrasonic disperse instrument, measures plasticizer DOP 20ml-80ml, epoxidized soybean oil (ESO) assisted class plasticizer 10ml-30ml mixing, through preparatory mechanical stirring and ultrasonic disperse Indwelling is spare after 30min-50min；
(3) it weighs: pressing mass fraction, weigh 100 parts of ABS resin raw material first；Measure the plasticizer 5 for being mixed with carbon nanotube - 10 parts of part；1 part -1.5 parts of weighing tetrapentaerythritol ester (antioxidant 1010)；Measure 0.5 part -1.5 parts of silane coupling agent；It weighs 0.1 part -0.5 part of chlorinated paraffin meter；Weigh 0.5 part -1.0 parts of aluminium hydroxide；
(4) it is stirred process: by ABS as high-speed mixer, being arranged -80 DEG C of temperature 60 C, revolving speed 700r/min-1000r/ Min, time 10min-30min sequentially add coupling agent, the plasticizer dissolved with enough carbon nanotubes, antioxidant, lubricant and resistance The functional aids such as agent are fired, continue to stir 10min-30min；
(5) melting extrusion mixes: thermoplastic resin matrix and function additive through high-speed stirred mixing are placed in screw extruder, into Row melting mixing is respectively set temperature (four sections): 160 DEG C -175 DEG C, 170 DEG C -185 DEG C, 180 DEG C -195 DEG C, 190 DEG C -210 DEG C, 185 DEG C -200 DEG C of nozzle, screw speed 25r/min-50r/min, then extruding pelletization is cooling, and pellet partial size is 3mm- 8mm, length 3mm-5mm, for use；
(6) injection molding process: by the pellet after melting mixing in 60 DEG C -85 DEG C dry 60min-120min, being added injection molding machine, Setting temperature: 165 DEG C -180 DEG C of ABS, 175 DEG C -190 DEG C, 185 DEG C -200 DEG C, 195 DEG C -220 DEG C, 190 DEG C -205 DEG C of spray head, Molten resin material is injected into preheated mold；Finally obtain the nano combined electromagnetic shielding material of resin base carbon.
Example IV
A kind of preparation method of the nano combined electromagnetic shielding material of resin base carbon, comprising the following steps:
(1) preparation of specific structure carbon nanotube: utilizing chemical vapour deposition technique (CVD), using methane as carbon-source gas, gas stream Amount is 100sccm-300sccm；Using argon gas as carrier gas, gas flow 200sccm-300sccm, reaction temperature 600 DEG C- Carbon nanotube is presented perpendicular to substrate in 800 DEG C, reaction time 1min-30min, catalyst Fe nano film thickness 1nm-5nm Array format growth, obtaining caliber is 10nm-20nm, and length is 15 μm -50 μm of vertical array column carbon nanotube；
(2) carbon nanotube preprocessing process: previously prepared carbon nanotube in (1) is peeled off from the substrate, and weighs 0.01g- 0.5g is scattered in it in dioctyl phthalate (DOP) plasticizer by ultrasonic disperse instrument, measures plasticizer DOP 10ml-100ml, indwelling is spare after preparatory mechanical stirring and ultrasonic disperse 20min-60min；
(3) it weighs: pressing mass fraction, weigh 100 parts of PE resin raw material first；Measure 5 parts of the plasticizer-for being mixed with carbon nanotube 10 parts；Weighing propionic acid octadecyl or 1,2 pairs 1 part -3 parts of hydrazine；Measure 0.5 part -2 parts of silane coupling agent；Weigh paraffin, chlorination stone Wax or 0.1 part -0.5 part of calcium stearate；Weighing weighing aluminium hydroxide, magnesium hydroxide or 0.5 part -1.0 parts of red phosphorus；
(4) it is stirred process: by PE as high-speed mixer, being arranged -80 DEG C of temperature 60 C, revolving speed 700r/min-1500r/ Min, time 10min-30min sequentially add coupling agent, the plasticizer dissolved with enough carbon nanotubes, antioxidant, lubricant and resistance The functional aids such as agent are fired, continue to stir 10min-30min；
(5) melting extrusion mixes: thermoplastic resin matrix and function additive through high-speed stirred mixing are placed in screw extruder, into Row melting mixing is respectively set temperature (four sections): 155 DEG C -165 DEG C, 165 DEG C -175 DEG C, 175 DEG C -185 DEG C, 185 DEG C -210 DEG C, 180 DEG C -195 DEG C of nozzle, screw speed 25r/min-50r/min, then extruding pelletization is cooling, and pellet partial size is 3mm- 8mm, length 3mm-5mm, for use.
(6) by the pellet after melting mixing in 60 DEG C -85 DEG C dry 60min-120min, note injection molding process: is added Molding machine, setting temperature: 60 DEG C -170 DEG C, 165 DEG C -180 DEG C, 170 DEG C -190 DEG C, 185 DEG C -205 DEG C, 180 DEG C -195 DEG C of spray head, Molten resin material is injected into preheated mold.Finally obtain the nano combined electromagnetic shielding material of resin base carbon.
The nano combined electromagnetic shielding shielding properties of resin base carbon is as shown in table 1:
The 1 nano combined electromagnetic shielding shielding properties of resin base carbon of table
Frequency point/Hz 150K 1M 30M 200M 450M 950M 1G 3G 8G 10G 18G
Shield effect/dB 32 40 57 55 60 56 60 40 49 51 41
Fig. 2 is multi-walled carbon nanotube TEM figure；Single-root carbon nano-tube transmission electron microscope photo, is shown as multi-walled carbon nanotube. Fig. 3 is that the multi-walled carbon nanotube SEM of specific length schemes；Array type multi-walled carbon nanotube shows strong point homogeneity, realizes carbon The length " cutting " of pipe, facilitates the dispersion in resin matrix.Fig. 4 is the nano combined electromagnetic shielding material sample of resin base carbon Outside drawing；Sample appearance flat array type carbon nanotube realizes good compound with resin matrix.Fig. 5 is that carbon nanotube is being set Distribution figure in aliphatic radical body.Fig. 6 is the nano combined electromagnetic shielding shielding properties of resin base carbon.Carbon nanotube is in resin matrix Good dispersion, composite material advantages of good shielding performance.
Only presently preferred embodiments of the present invention is explained in detail above, but the present invention is not limited to above-described embodiment, Within the knowledge of a person skilled in the art, it can also make without departing from the purpose of the present invention each Kind variation, various change should all be included in the protection scope of the present invention.

Claims (10)

1. a kind of nano combined electromagnetic shielding material of resin base carbon, it is characterised in that: including thermoplastic resin and carbon nanotube, institute Carbon nanotube is stated using vertical array column carbon nanotube；It disperses orthogonal array carbon nanotube in thermoplastic resin matrix, Electromagnetic shielding material is made by mixed at high speed, Shooting Technique.
2. a kind of preparation method of the nano combined electromagnetic shielding material of resin base carbon, which comprises the following steps:
The preparation of S1, vertical array column carbon nanotube: utilizing chemical vapour deposition technique, and obtaining caliber is 10nm-20nm, and length is 10 μm -200 μm of vertical array column carbon nanotube；
S2, carbon nanotube preprocessing process: the vertical array column carbon nanotube prepared in S1 is peeled off from the substrate, and is weighed It is spare to measure plasticizer 10ml-100ml indwelling after preparatory mechanical stirring and ultrasonic disperse 20min-60min by 0.01g-1g；
S3, weighing: pressing mass fraction, weighs 100 parts of thermoplastic resin raw materials；Measure 5 parts of the plasticizer-for being mixed with carbon nanotube 20 parts；Weigh 1 part -3 parts of antioxidant；Measure 0.5 part -2 parts of silane coupling agent；Weigh 0.1 part -0.5 part of lubricant；Weigh hydrogen-oxygen Change one of aluminium, magnesium hydroxide and red phosphorus or a variety of 0.5 part -1.5 parts of mixing；
S4, it is stirred process: by thermoplastic resin raw materials as high-speed mixer, being arranged -80 DEG C of temperature 60 C, revolving speed 700r/min-1500r/min, time 10min-30min sequentially add coupling agent, the plasticizer, anti-dissolved with enough carbon nanotubes Oxygen agent, lubricant and fire retardant continue to stir 10min-30min；
S5, melting extrusion mixing: thermoplastic resin matrix and function additive through high-speed stirred mixing are placed in screw extruder, into Row melting mixing is granulated after squeezing out, and pellet partial size is 3mm-8mm, length 3mm-5mm；
S6, injection molding process: by pellet in S5 in 60 DEG C -85 DEG C dry 60min-120min, injection molding machine is added, finally obtains The nano combined electromagnetic shielding material of resin base carbon.
3. a kind of preparation method of nano combined electromagnetic shielding material of resin base carbon according to claim 2, feature exist In: the carbon nanotube chemical vapor deposition processes, using methane or ethylene as carbon-source gas, gas flow 100sccm- 300sccm；Using argon gas as carrier gas, gas flow 200sccm ~ 300sccm；Using iron nano-film as catalyst, film is thick Degree is 1nm-5nm；Reaction temperature is 600 DEG C -800 DEG C；Reaction time is 1min-30min.
4. a kind of preparation method of nano combined electromagnetic shielding material of resin base carbon according to claim 2, feature exist In: the plasticizer uses phthalic ester plasticizer；Or aliphatic is aided with using phthalic ester plasticizer Binary acid ester plasticizer or epoxy ester series plasticizer mixed form.
5. a kind of preparation method of nano combined electromagnetic shielding material of resin base carbon according to claim 4, feature exist In: the phthalic ester plasticizer is dioctyl phthalate or diisooctyl phthalate；The aliphatic Binary acid ester plasticizer is dioctyl adipate；The epoxy ester series plasticizer is epoxidized soybean oil.
6. a kind of preparation method of nano combined electromagnetic shielding material of resin base carbon according to claim 2, feature exist In: the antioxidant is tetrapentaerythritol ester, propionic acid octadecyl, 1, one of 2 pairs of hydrazines.
7. a kind of preparation method of nano combined electromagnetic shielding material of resin base carbon according to claim 2, feature exist In: the lubricant is one of paraffin, chlorinated paraffin, calcium stearate.
8. a kind of preparation method of nano combined electromagnetic shielding material of resin base carbon according to claim 2, feature exist In: the thermoplastic resin raw materials are one of polypropylene, polyethylene, ABS plastic.
9. a kind of preparation method of nano combined electromagnetic shielding material of resin base carbon according to claim 8, feature exist In: when the thermoplastic resin raw materials are polypropylene or polyethylene, when melting mixing squeezes out, screw extruder temperature setting is 155 DEG C -165 DEG C, 165 DEG C -175 DEG C, 175 DEG C -185 DEG C, 185 DEG C -210 DEG C, 180 DEG C -195 DEG C of nozzle；The thermoplastic resin Fat raw material be ABS plastic when, melting mixing squeeze out when, screw extruder temperature setting be 160 DEG C -175 DEG C, 170 DEG C -185 DEG C, 180 DEG C -195 DEG C, 190 DEG C -210 DEG C, 185 DEG C -200 DEG C of nozzle；Screw extruder screw speed is 25r/min-50r/min.
10. a kind of preparation method of nano combined electromagnetic shielding material of resin base carbon according to claim 8, feature exist In: when the thermoplastic resin raw materials are polypropylene or polyethylene, injection temperature is 160 DEG C -170 DEG C, 165 DEG C -180 DEG C, 170 DEG C -190 DEG C, 185 DEG C -205 DEG C, 180 DEG C -195 DEG C of spray head；When the thermoplastic resin raw materials are ABS plastic, injection temperature is 165 DEG C -180 DEG C, 175 DEG C -190 DEG C, 185 DEG C -200 DEG C, 195 DEG C -220 DEG C, 190 DEG C -205 DEG C of spray head.
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CN115584119A (en) * 2022-11-11 2023-01-10 成都佳驰电子科技股份有限公司 Corrosion-resistant light high-conductivity carbon-system flexible conductive shielding film and preparation method thereof

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Application publication date: 20191115