CN100539821C - The preparation method of carbon nano-tube nonwoven cloth electromagnetic shielding composite material - Google Patents
The preparation method of carbon nano-tube nonwoven cloth electromagnetic shielding composite material Download PDFInfo
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- CN100539821C CN100539821C CNB2007101951057A CN200710195105A CN100539821C CN 100539821 C CN100539821 C CN 100539821C CN B2007101951057 A CNB2007101951057 A CN B2007101951057A CN 200710195105 A CN200710195105 A CN 200710195105A CN 100539821 C CN100539821 C CN 100539821C
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Abstract
The present invention relates to a kind of preparation method who electromagnetic wave is had the Single Walled Carbon Nanotube nonwoven cloth electromagnetic shielding composite material of screen effect.The present invention with the Single Walled Carbon Nanotube nonwoven fabrics as conductive filler, with fluoropolymer resin as basis material, getting previously prepared Single Walled Carbon Nanotube nonwoven fabrics is immersed in the ethanol, treat that it soaks into the back fully and takes out, put it into rapidly in the deionized water, treat that the Single Walled Carbon Nanotube nonwoven fabrics spreads on the water surface fully after, the carbon nano-tube non-woven fabrics after soaking into is transferred in the mould that scribbles remover, vacuumize, standby; Thermosetting resin 100 ℃ of following vacuum degassings 1 hour, is poured in the mould that is covered with carbon nano-tube non-woven fabrics and solidified the demoulding.
Description
Technical field
The present invention relates to a kind of preparation method who electromagnetic wave is had the Single Walled Carbon Nanotube nonwoven cloth electromagnetic shielding composite material of screen effect.
Background technology
Electromagnetic Interference is meant that harmful electromagnetic wave is interfered the normal function of electronic device or causes the phenomenon of obstacle, be called for short EMI (electromagnetic interference), general reference radio wave, magnetic wave, light wave, sunspot and some other natural disturbance from the space.Along with a large amount of the popularizing of the high speed development of hyundai electronics industry and various commercialization and domestic electronic, electric equipment products such as computer, mobile phone used, electromagenetic wave radiation of Chan Shenging and electromagnetic interference are serious day by day therefrom, have become a kind of new social effects of pollution.On the one hand, the electromagnetic radiation meeting causes serious interference to electronic equipment on every side, and their working procedure is got muddled, and produces malfunction; And electromagenetic wave radiation can cause leakage of information, and the information security of instruments such as computer is seriously influenced.Find that now electromagnetic radiation not only has interference to electronic device, also can produce harm to human body.The raising of disease incidence such as cancer, leukaemia and the increase of electromagnetic radiation have certain relation.At present, how international organization and national governments, scientific research circle etc. are to preventing Electromagnetic Interference to give great attention. and formulated strict rules and come trapped electromagnetic wave radiation capacity.As the FCC standard that the U.S. implements nineteen eighty-three, international standard and test method that the international wireless reactance disturbs special committee (CISPR) also to make the anti-electromagnetic wave interference are consulted and carried out for various countries.Be interference and the leakage that prevents that electromagenetic wave radiation from causing, adopting electromagnetic shielding material to shield is main method.Traditional electromagnetic shielding material mostly is metal material or ferrite powders such as Cu, Ag, Fe, Ni, is dispersed in polymer as obtaining in the basis materials such as silicon rubber, Merlon or epoxy resin.Metal material has higher conductivity and excellent mechanical property, but its density is big, perishable, difficult processing, and limitation is bigger.Therefore in recent years, realize that as conductive filler the electromagnetic shielding characteristic of material also has report by dosing carbon nano-tube, but all there are some common problems in these methods.At first, thereby to form conductivity that conductive network makes composite material and improve and reach desirable shield effectiveness in order to overlap mutually in basis material, the amount of filling of needed conductive filler is all very high, dose about 10%wt even higher.The dispersion of the functional material of being dosed in matrix is the main cause of the resulting composite material character of influence, and filler can have influence on the character of matrix itself, brings the decline of matrix mechanical property, process conditions complicated.And because amount of filling is generally higher, and the filler of being dosed mostly is nontransparent, therefore, the transparency of composite material can be subjected to very big influence and can not satisfy some specific (special) requirements.It is a lot of that added filler can make the weight of composite material increase, and dispersion need be carried out surface treatment or dose surfactant, and this has increased technology difficulty, and make last handling process become complicated more.Therefore, need a kind of conductive filler amount of filling few, shield effectiveness is high and can keep electromagnetic shielding material than high transparent.
Summary of the invention
The purpose of this invention is to provide a kind of in light weight, shield effectiveness is high and can keep preparation method than the Single Walled Carbon Nanotube nonwoven cloth electromagnetic shielding composite material of high transparent.Technical solution of the present invention is, with the Single Walled Carbon Nanotube nonwoven fabrics as conductive filler, with fluoropolymer resin as basis material, getting previously prepared Single Walled Carbon Nanotube nonwoven fabrics is immersed in the ethanol, treat that it soaks into the back fully and takes out, put it into rapidly in the deionized water, treat that carbon nano-tube non-woven fabrics spreads on the water surface fully after, composite polymeric resin one of as follows:
(1) carbon nano-tube non-woven fabrics after will soaking into is transferred in the mould that scribbles remover, and vacuumize is standby; Thermosetting resin 100 ℃ of following vacuum degassings 1 hour, is poured in the mould that is covered with carbon nano-tube non-woven fabrics and solidified the demoulding;
(2) carbon nano-tube non-woven fabrics is transferred on the thermoplastic resin diaphragm of 100 ℃ of preliminary treatment 12h in baking oven, thermoplastic resin diaphragm with the same size of other a slice covers on the carbon nano-tube non-woven fabrics again, insert then to be put in the anchor clamps that scribble remover and carry out hot-pressing processing on the hot-platen, the hot-platen temperature is about 350 ℃, pressure maintains 10kN, continue pressurize 10min, treat that hot-platen naturally cools to room temperature after, the composite material after the compression process is taken out from mould;
(3) carbon nano-tube non-woven fabrics is transferred on the sheet glass that scribbles remover in advance, after the vacuumize, drip thermosetting resin in the nanotube nonwoven surface, treat that thermosetting resin is after the nanotube nonwoven surface spreads fully, the sheet glass that other a slice is scribbled remover covers its surface, after the curing that heats up in baking oven sheet glass is taken off.
Described thermoplastic resin is meant silicon rubber or polypropylene or polymethyl methacrylate or polyvinyl alcohol or polyether-ether-ketone.
Described thermosetting resin is meant epoxy resin, bimaleimide resin or thermoset polyimide resin or phenolic resins or cyanate ester resin or unsaturated polyester resin.
As the thickness of the Single Walled Carbon Nanotube nonwoven fabrics of conductive filler according to the requirement of electromagnetic shielding efficiency from 100nm to 1 μ m.
The advantageous effect that the present invention has: the Single Walled Carbon Nanotube nonwoven fabrics consumption as conductive filler is very low, and be with a global existence independently, need not special processing can be directly and basis material compound, the scattering problem of filler in matrix that has existed when having avoided selecting other powder conductive fillers for use.And carbon nano-tube non-woven fabrics itself is a kind of independently monolithic film membrane material that is cross-linked with each other in growth course and is formed together by Single Walled Carbon Nanotube, and its conductivity will be far above the formed conductive network of powder conductive filler.The electromagnetic shielding characteristic of composite material only derives from carbon nano-tube non-woven fabrics, and is irrelevant with matrix resin, therefore only needs single-layer carbon nano-tube non-woven fabrics just can realize the electromagnetic shielding effect of composite material.And the pliability of carbon nano-tube non-woven fabrics is fine, with thermal plastic high polymer and silicon rubber compound after, can arbitrarily be folded into Any shape, be fit to the preparation of the microminiature parts of special shape.And composite material low-frequency band (electromagnetic shielding efficiency of 10MHz～1.5GHz)〉20dB.
Embodiment
With carbon nano-tube non-woven fabrics as conductive filler, with fluoropolymer resin as basis material, getting previously prepared carbon nano-tube non-woven fabrics is immersed in the ethanol, name of document is " a kind of single-layer carbon nano-tube non-woven fabrics and preparation method thereof " (Direct Synthesis ofa Macroscale Single-walled Carbon Nanotube Non-Woven Material on employing Germany " advanced material " magazine, Adv.Mater.2004,16, (17) 1529-1534) preparation method who is reported in prepares carbon nano-tube non-woven fabrics.Because the diffusion of ethanol molecule in water and the hydrophobicity of nonwoven fabrics itself of carbon nano-tube non-woven fabrics absorption, nonwoven fabrics will spread on the water surface fully, treat that it soaks into the back fully and takes out, put it in the deionized water rapidly, after treating that carbon nano-tube non-woven fabrics spreads on the water surface fully, composite polymeric resin one of as follows:
(1) carbon nano-tube non-woven fabrics after will soaking into is transferred in the mould that scribbles remover, and vacuumize is standby; Thermosetting resin 100 ℃ of following vacuum degassings 1 hour, is poured in the mould that is covered with carbon nano-tube non-woven fabrics and solidified the demoulding;
(2) carbon nano-tube non-woven fabrics is transferred in baking oven on 12 hours the thermoplastic resin diaphragm of 100 ℃ of preliminary treatment, thermoplastic resin diaphragm with the same size of other a slice covers on the carbon nano-tube non-woven fabrics again, insert then to be put in the anchor clamps that scribble remover and carry out hot-pressing processing on the hot-platen, the hot-platen temperature is about 350 ℃, pressure maintains 10kN, continue pressurize 10min, treat that hot-platen naturally cools to room temperature after, the composite material after the compression process is taken out from mould;
(3) carbon nano-tube non-woven fabrics is transferred on the sheet glass that scribbles remover in advance, after the vacuumize, drip thermosetting resin in the nanotube nonwoven surface, treat that fluoropolymer resin is after the nanotube nonwoven surface spreads fully, the sheet glass that other a slice is scribbled remover covers its surface, after the curing that heats up in baking oven sheet glass is taken off.
Described thermoplastic resin is meant silicon rubber or polypropylene or polymethyl methacrylate or polyvinyl alcohol or polyether-ether-ketone.
Described thermosetting resin is meant epoxy resin, bimaleimide resin or thermoset polyimide resin or phenolic resins or cyanate ester resin or unsaturated polyester resin.
As the thickness of the Single Walled Carbon Nanotube nonwoven fabrics of conductive filler according to the requirement of electromagnetic shielding efficiency from 100nm to 1 μ m.
Embodiment one:
The carbon nano-tube non-woven fabrics that with thickness is 200nm prepares electromagnetic shielding material as conductive filler.Getting previously prepared nonwoven fabrics is immersed in the ethanol, treat that it soaks into the back fully and takes out, put it in the deionized water rapidly, because the diffusion of ethanol molecule in water and the hydrophobicity of nonwoven fabrics itself of carbon nano-tube non-woven fabrics absorption, nonwoven fabrics will spread on the water surface fully, then it is transferred in the mould that scribbles remover in advance that depth of groove is 0.5mm, vacuumize, standby.At 1 hour epoxy resin of 100 ℃ of following vacuum degassings, pour in the mould that is covered with carbon nano-tube non-woven fabrics and solidify the demoulding.
Prepared composite material is carried out the spectrum transmitting experiment, find that composite material has higher permeability at visible light and near infrared light zone.Composite material is carried out the test of electromagnetic shielding efficiency and find that the electromagnetic shielding efficiency of composite material reduces with the increase of wave frequency, but it still has higher electromagnetic shielding efficiency at the low frequency electromagnetic wave band.To frequency is that the electromagnetic wave shielding efficient of 10MHz is 30dB, is the electromagnetic shield effectiveness that still can keep 26dB of 1.5GHz to frequency.
Embodiment two:
The carbon nano-tube non-woven fabrics that with thickness is 100nm prepares electromagnetic shielding material as conductive filler.Spread over carbon nano-tube non-woven fabrics on the water surface fully as embodiment 1 described method, it is transferred to thickness 50 μ m and in advance in baking oven on 12 hours polyether-ether-ketone of 100 ℃ of preliminary treatment (PEEK) diaphragm, with the polyether-ether-ketone membrane covered of the same size of other a slice on nonwoven fabrics.The composite bed of this " sandwich " structure is inserted be put in the anchor clamps that scribble remover then and carry out hot-pressing processing on the hot-platen.In the experiment of pressing process, the hot-platen temperature is that pressure maintains 10kN about 350 ℃, continues pressurize 10min.After treating that hot-platen naturally cools to room temperature, the composite material after the compression process is taken out from mould.To its carry out electromagnetic shielding efficiency test find to embodiment 1 in prepared epoxy resin/carbon nano-tube non-woven fabrics composite material have similar result.
Embodiment three:
With thickness is that the carbon nano-tube non-woven fabrics of 1 μ m prepares electromagnetic shielding material as conductive filler.Spread over carbon nano-tube non-woven fabrics on the water surface fully as embodiment 1 described method, then it is transferred in the mould that scribbles remover in advance that depth of groove is 0.5mm, after the vacuumize, (monomer is a hydroxyl-terminated injecting two methyl siloxane with silicon rubber, curing agent is an ethyl orthosilicate) pour in the mould, after solidifying 3h under the room temperature, laminated film is taken off, because good pliability and the operability of carbon nano-tube non-woven fabrics itself, can not have influence on the soft characteristic of silicon rubber matrix own, can arbitrarily bend to Any shape, can be used for preparing the microminiature part of some special shapes that need have electromagnetic shielding characteristic.Prepared silicon rubber/carbon nano-tube non-woven fabrics composite material is carried out the electromagnetic shielding efficiency test, can obtain and the similar result of composite material described in the embodiment 1.
Embodiment four:
The carbon nano-tube non-woven fabrics that with thickness is 500nm prepares electromagnetic shielding material as conductive filler.Spread over carbon nano-tube non-woven fabrics on the water surface fully as embodiment 1 described method, it is transferred on the sheet glass that scribbles remover in advance then, after the vacuumize, drip epoxy resin in nonwoven surface, treat that epoxy resin is after nonwoven surface spreads fully, the sheet glass that scribbles remover that other a slice is onesize covers its surface, intensification after solidifying is taken laminated film off in baking oven, this electromagnetic wave shield film can be trimmed to the shape of various needs, stick on device surface by epoxy adhesive, thereby and can realize that different shield effectivenesses satisfies different components by the number of plies of shielded film, the requirement of different parts electromagnetic shielding efficiency.
Claims (4)
1. the preparation method of a Single Walled Carbon Nanotube nonwoven cloth electromagnetic shielding composite material, it is characterized in that, with the Single Walled Carbon Nanotube nonwoven fabrics as conductive filler, with fluoropolymer resin as basis material, get previously prepared Single Walled Carbon Nanotube nonwoven fabrics and be immersed in the ethanol, treat that it soaks into the back fully and takes out, and puts it in the deionized water rapidly, after treating that the Single Walled Carbon Nanotube nonwoven fabrics spreads on the water surface fully, composite polymeric resin one of as follows:
(1) carbon nano-tube non-woven fabrics after will soaking into is transferred in the mould that scribbles remover, and vacuumize is standby; Thermosetting resin 100 ℃ of following vacuum degassings 1 hour, is poured in the mould that is covered with carbon nano-tube non-woven fabrics and solidified the demoulding;
(2) carbon nano-tube non-woven fabrics is transferred on the thermoplastic resin diaphragm of 100 ℃ of preliminary treatment 12h in baking oven, thermoplastic resin diaphragm with the same size of other a slice covers on the carbon nano-tube non-woven fabrics again, insert then to be put in the anchor clamps that scribble remover and carry out hot-pressing processing on the hot-platen, the hot-platen temperature is about 350 ℃, pressure maintains 10kN, continue pressurize 10min, treat that hot-platen naturally cools to room temperature after, the composite material after the compression process is taken out from mould;
(3) carbon nano-tube non-woven fabrics is transferred on the sheet glass that scribbles remover in advance, after the vacuumize, drip thermosetting resin on the carbon nano-tube non-woven fabrics surface, treat that thermosetting resin is after spread fully on the carbon nano-tube non-woven fabrics surface, the sheet glass that other a slice is scribbled remover covers its surface, after the curing that heats up in baking oven sheet glass is taken off.
2. the preparation method of Single Walled Carbon Nanotube nonwoven cloth electromagnetic shielding composite material according to claim 1 is characterized in that, described thermoplastic resin is meant silicon rubber or polypropylene or polymethyl methacrylate or polyvinyl alcohol or polyether-ether-ketone.
3. the preparation method of Single Walled Carbon Nanotube nonwoven cloth electromagnetic shielding composite material according to claim 1, it is characterized in that described thermosetting resin is meant epoxy resin, bimaleimide resin or thermoset polyimide resin or phenolic resins or cyanate ester resin or unsaturated polyester resin.
4. the preparation method of Single Walled Carbon Nanotube nonwoven cloth electromagnetic shielding composite material according to claim 1 is characterized in that, as the thickness of the carbon nano-tube non-woven fabrics of conductive filler according to electromagnetic shielding efficiency from 100nm to 1 μ m.
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| CNB2007101951057A CN100539821C (en) | 2007-11-29 | 2007-11-29 | The preparation method of carbon nano-tube nonwoven cloth electromagnetic shielding composite material |
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| CNB2007101951057A CN100539821C (en) | 2007-11-29 | 2007-11-29 | The preparation method of carbon nano-tube nonwoven cloth electromagnetic shielding composite material |
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| CN100539821C true CN100539821C (en) | 2009-09-09 |
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| CN101998817A (en) * | 2009-08-12 | 2011-03-30 | 鸿富锦精密工业（深圳）有限公司 | Anti-electromagnetic interference molding piece and preparation method thereof |
| CN102378560B (en) * | 2010-08-18 | 2015-05-20 | 富葵精密组件(深圳)有限公司 | Film having electromagnetic shielding effect and manufacturing method thereof |
| CN102378561B (en) * | 2010-08-19 | 2015-05-20 | 富葵精密组件(深圳)有限公司 | Covering membrance with electromagnetic shielding function and manufacturing method of covering membrance |
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| CN102250327B (en) * | 2011-04-08 | 2013-02-13 | 同济大学 | Method for preparing carbon nanotube-containing aromatic thermosetting resin |
| CN102516569B (en) * | 2011-11-18 | 2014-05-14 | 中国航空工业集团公司北京航空材料研究院 | Preparation method for carbon nanotube non-woven fabric interlayer modified fiber reinforced composite materials |
| CN102704351B (en) * | 2012-05-18 | 2014-10-22 | 中国航空工业集团公司北京航空材料研究院 | Preparation method of carbon nano tube non-woven fabrics |
| CN103088462B (en) * | 2013-01-30 | 2015-01-07 | 吉林大学 | Preparation method of polyether-ether-ketone monofilament with electromagnetic shielding function |
| CN104059464B (en) * | 2013-03-20 | 2016-05-18 | 中国科学院上海硅酸盐研究所 | Composition and coating and method for Electromagnetism Shield Composite Coating |
| CN105086463A (en) * | 2014-05-20 | 2015-11-25 | 深圳光启高等理工研究院 | Composite absorbing material, preparation method and application thereof |
| CN105255383A (en) * | 2015-09-25 | 2016-01-20 | 常熟华尚新材料科技有限公司 | Stratified electromagnetic shielding material containing carbon nanotube network resin base, and preparation method thereof |
| CN108749194A (en) * | 2018-08-30 | 2018-11-06 | 天津工业大学 | A kind of electromagnetic shielding sandwich laminated film and preparation method thereof |
| US20220071068A1 (en) * | 2019-01-28 | 2022-03-03 | Zeon Corporation | Electromagnetic wave absorbing sheet |
| CN110819108A (en) * | 2019-11-23 | 2020-02-21 | 西北工业大学 | Polyimide/carbon nanotube electromagnetic shielding composite material with isolation structure |
| CN111552381A (en) * | 2020-04-23 | 2020-08-18 | 中国科学院半导体研究所 | Capacitive pressure sensor, preparation method thereof and piano gloves |
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