CN102181912A - Method for preparing nano polymer composite material based on electrophoretic deposition - Google Patents
Method for preparing nano polymer composite material based on electrophoretic deposition Download PDFInfo
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Abstract
The invention discloses a method for preparing a nano polymer composite material based on electrophoretic deposition in the technical field of nano materials. The technical scheme comprises the following steps of: mixing a carbon nanotube or a carbon nanofiber and a surfactant; adding water into the mixture to obtain carbon nano electrophoretic suspension; mixing the suspension and a cured anode electrophoretic coating or cathode electrophoretic coating; and performing electrophoretic deposition and curing treatment to obtain the nano polymer composite material. By the preparation method, the carbon nanotube/carbon nanofiber in the prepared composite material has high dispersibility in polymer and can be preferably combined with the polymer, and the performance of the original polymer is effectively improved.
Description
Technical field
What the present invention relates to is a kind of method of technical field of nano material, specifically is a kind of preparation method based on the electrophoretic deposition nano-polymer composite material.
Background technology
Since Japanese scientist Iijima in 1991 found carbon nanotube, carbon nanotube had become the focus of people's research with its excellent mechanics, calorifics, magnetics and electric property.As material modified matrix material big quantity research has been arranged with carbon nano-tube/carbon nano fabric over the last couple of decades, as metal matrix carbon nano-tube/carbon nano fabric matrix material, polymer-base carbon nanotube/carbon nano-fiber composite material.Can prepare metal matrix carbon nano-tube/carbon nano fabric matrix material by composite electric plating method, along with the mechanical property of the adding matrix material of carbon nano-tube/carbon nano fabric has had tangible improvement.
At present about the research of carbon nano-tube/carbon nano fabric polymer composites mainly concentrate on carbon nano-tube/carbon nano fabric improve the mechanics, electric property of matrix material and with matrix material as sensing material.Because carbon nano-tube/carbon nano fabric has excellent mechanical property, adopt carbon nano-tube/carbon nano fabric as packing material, the mechanical property of matrix material (as tensile strength, impelling strength, aging intensity etc.) can obtain the improvement of certain degree, and thermostability, hardness all improve greatly.Carbon nano-tube/carbon nano fabric has high conductivity and high length-to-diameter ratio, adding small amount of carbon nanotubes/carbon nanofiber can increase substantially the electroconductibility of material, has huge application potential in composite conducting polymer material, antistatic material and electromagnetic shielding material field.Therefore preparing the carbon nano-tube/carbon nano fabric polymer composites has very tempting application prospect, mainly be to adopt melt-blending process at present, solution blended process, preparation such as situ aggregation method carbon nano-tube/carbon nano fabric polymer composites, significant variation has taken place in prepared mechanics of composites, calorifics, electric property etc.
Electrophoresis is the phenomenon that charged particle or molecule move in extra electric field, electrophoretic deposition has plentiful, even, smooth, the slick advantage of coating, and the hardness of electrodeposited paint film, sticking power, corrosion resistant, impact property, penetrating quality obviously are better than other coating process.Electrophoresis deposition of carbon nanotubes/carbon nanofiber is a kind of effective method for preparing the carbon nano-tube/carbon nano fabric film on the matrix of conduction, the homodisperse carbon nano-tube/carbon nano fabric is the key of electrophoretic deposition carbon nano-tube/carbon nano fabric in stable solvent, it can be in complex-shaped substrate deposit film, the prepared film even compact combines with substrate well, has been used for feds, fuel cell, ultracapacitor etc. at present.(the W.B.Choi such as W.B.Choi of Samsung company, etl.Electrophoresis deposition of carbon nanotubes for triode-type field emission display[J] .APPLIED PHYSICS LETTERS, 2001,78:1547-1549.) to adopt the electrophoretic deposition carbon nanotube be emission three an electrode indicating meter, the simple and reliable field of preparation method launching effect is good.
Electrophoretic deposition carbon nano-tube/carbon nano fabric aspect mainly concentrates on deposition single carbon nanotube/carbon nanofiber thin-film material at present with the preparation functional film, as is applied to feds, ultracapacitor and gas sensor etc. in the domestic and international research.Because the advantage of electrophoretic deposition, as be easy on the matrix of complicated shape deposition preparation matrix material, prepared thickness of composite material speed is controlled, thereby adopts the method for electrophoretic deposition that a kind of effective way of novelty is provided for preparation carbon nano-tube/carbon nano fabric polymer composites.
Summary of the invention
The present invention is directed to the prior art above shortcomings, a kind of preparation method based on the electrophoretic deposition nano-polymer composite material is provided, carbon nano-tube/carbon nano fabric favorable dispersity and polymkeric substance in polymkeric substance improved original polymer properties effectively in conjunction with better in the prepared matrix material.
The present invention is achieved by the following technical solutions, the present invention by with carbon nanotube or carbon nanofiber with add water after tensio-active agent mixes and obtain carbon nanometer electrophoresis suspensioning liquid, then with maturation process after anode electrophoresis dope or cathode electrophoresis dope mixes after electrophoretic deposition and solidification treatment obtain nano-polymer composite material.
Described carbon nanotube or carbon nanofiber through too shortly cut, purifying modifies and handles, specifically be meant: with ball mill to carbon nanotube or carbon nanofiber to carrying out ball-milling processing, ball milling speed 100-6000rpm, ball milling time-300min, be 1 in volume ratio then: 9-9: in 1 the vitriol oil and the mixed acid solution of concentrated nitric acid 50-120 ℃ following reflow treatment 1-12 hour, postcooling to the room temperature of finishing dealing with is neutral with a large amount of deionized water wash until solution.
The described vitriol oil and concentrated nitric acid are respectively massfractions greater than 70% sulphuric acid soln and massfraction greater than 65% salpeter solution.
Described tensio-active agent is cats product, anion surfactant or nonionogenic tenside.
Described maturation process is meant mixes anode electrophoresis dope or cathode electrophoresis dope and water by mass ratio 0.2-5, again through sonic oscillation and the polymer coating electrophoresis suspensioning liquid that obtains more than the mechanical stirring 12h.
The mass ratio of described carbon nanometer electrophoresis suspensioning liquid and anode electrophoresis dope or cathode electrophoresis dope is 0.2-5.
Described electrophoretic deposition is meant: electrophoretic voltage 40-200V, interelectrode distance 1-10cm, electrophoretic deposition time 30-300s, electrophoresis suspensioning liquid temperature are 25-35 ℃ under DC mode and constant voltage, and the effect of electric field lower surface has the carbon nanotube of like charges or carbon nanofiber and polymer molecule together to the opposite electrode swimming of charge property outside.
Described solidification treatment is meant: toast 30-120min under 120-200 ℃ of environment.
The invention has the advantages that:
(1) adopts the carbon nano-tube/carbon nano fabric polymer composites growth velocity of electrophoretic deposition method preparation controlled, is easy to realize the described matrix material of deposition on graphical, as the to be adapted at complicated shape matrix; (2) introducing its physical strength behind the carbon nano-tube/carbon nano fabric, toughness, heat conductivility in the polymkeric substance may obviously improve; (3) conductivity of matrix material such as specific conductivity also significantly raise, and it is all having good prospects for application aspect static release, the electromagnetic shielding.
Description of drawings
The electrophoretic deposition synoptic diagram of Fig. 1 carbon nano-tube/carbon nano fabric polymer composites;
The carbon nano-tube/carbon nano fabric polymer composites of Fig. 2 electrophoretic deposition preparation is organized synoptic diagram;
Among the figure: 1 direct supply, 2 anodes, 3 negative electrodes, 4 carbon nanotubes or carbon nanofiber, 5 polymer molecules, 6 carbon nanotubes or carbon nanofiber polymer composites, 7 electrophoresis chambers, 8 extra electric fields.
Among Fig. 2: 9 carbon nanotubes or carbon nanofiber, 2 polymer molecules.
Embodiment
Below embodiments of the invention are elaborated, present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
(1) takes by weighing the 2g Single Walled Carbon Nanotube, in ball mill with the rotating speed ball milling 3h of 3000rpm, then the carbon nanotube behind the ball milling is dispersed in the mixed acid solution of the 400ml vitriol oil/concentrated nitric acid (volume ratio is 1: 1), and at 60 ℃ of following reflow treatment 4h, be neutral with a large amount of deionized water wash until solution again, at last 80 ℃ of following drying treatment 24h in vacuum drying oven.
(2) get above-mentioned carbon nanotube 1g and be dispersed in the 200ml water, add 1g cats product cetyl trimethyl bromine ammonium (CTAB) again, sonic oscillation 1h obtains dispersed good carbon nano tube suspension behind the mechanical stirring 10min.
(3) will 100g epoxy acrylic cathode electrophoresis dope and the 200ml deionization be mixed with suspension after mixing, induction stirring 12h behind (25 ℃) sonic oscillation 1h at room temperature obtains the epoxy acrylic cathode electrophoresis dope suspension of slaking.
(4) electrophoresis suspensioning liquid in the carbon nano tube suspension described in (2) and (3) is mixed, at 32 ℃ of following thermostatic ultrasonic vibration 30min.
(5) insert two electrodes respectively as anode and negative electrode in the electrophoresis suspensioning liquid described in (4), anode and negative electrode are stainless steel plate; Electrophoretic deposition under DC mode, keeping two interelectrode distances is that 5cm, electrophoretic voltage are that 120V, electrophoresis time are 30s, treat electrophoresis finish after in deionized water residual electrophoresis suspensioning liquid on the flush away electrode.
(6) carbon nanotube/epoxy acrylic matrix material with electrophoretic deposition is drying 1h naturally in air, and 200 ℃ of curing 30min in vacuum drying oven promptly obtain final carbon nanotube/epoxy acrylic matrix material again.
(7) in prepared carbon nanotube/epoxy acrylic matrix material, content of carbon nanotubes is about 0.4%, and epoxy acrylic accounts for 99.6%, and salt-fog resistant time is greater than 1200h, and acid resistance and alkali resistance all reach more than the 24h, and corrosion resistance nature is preferably arranged.
(1) takes by weighing the 2g carbon nanofiber, in ball mill with the rotating speed ball milling 2h of 6000rpm, then the carbon nanofiber behind the ball milling is dispersed in the mixed acid solution of the 600ml vitriol oil/concentrated nitric acid (volume ratio is 2: 1), and at 80 ℃ of following reflow treatment 3h, be neutral with a large amount of deionized water wash until solution again, at last 100 ℃ of following drying treatment 24h in vacuum drying oven.
(2) get above-mentioned carbon nanofiber 1g and be dispersed in the 200ml water, add 0.5g cats product cetyl trimethyl bromine ammonium (CTAB) again, sonic oscillation 1h behind the mechanical stirring 10min obtains dispersed good carbon nanofiber suspension.
(3) will the polyamide modified Resins, epoxy electrophoretic paint of 100g hard and the 200ml deionization be mixed with suspension after mixing, induction stirring 12h behind (25 ℃) sonic oscillation 1h at room temperature obtains the polyamide modified Resins, epoxy electrophoretic paint of the hard suspension of slaking.
(4) electrophoresis suspensioning liquid in the carbon nanofiber suspension described in (2) and (3) is mixed, at 30 ℃ of following sonic oscillation 30min.
(5) insert two electrodes respectively as anode and negative electrode in the electrophoresis suspensioning liquid described in (4), anode and negative electrode are stainless steel plate; Electrophoretic deposition under DC mode, keeping two interelectrode distances is that 2cm, electrophoretic voltage are that 80V, electrophoresis time are 120s, treat electrophoresis finish after in deionized water residual electrophoresis suspensioning liquid on the flush away electrode.
(6) the polyamide modified epoxy resin composite material of the carbon nanofiber/hard of electrophoretic deposition is being dried 1h naturally in air, 180 ℃ of curing 60min in vacuum drying oven promptly obtain the polyamide modified epoxy resin composite material of final carbon nanofiber/hard again.
(7) in the prepared polyamide modified epoxy resin composite material of carbon nanofiber/hard, carbon nanofiber content is about 0.5%, the polyamide modified Resins, epoxy of hard accounts for 99.5%, salt-fog resistant time is greater than 1300h, acid resistance and alkali resistance all reach more than the 24h, and corrosion resistance nature is preferably arranged.
(1) takes by weighing 1g Single Walled Carbon Nanotube and 1g multi-walled carbon nano-tubes, in ball mill with the rotating speed ball milling 8h of 1000rpm, then the carbon nanotube behind the ball milling is dispersed in the mixed acid solution of the 600ml vitriol oil/concentrated nitric acid (volume ratio is 3: 1), and at 100 ℃ of following reflow treatment 2h, be neutral with a large amount of deionized water wash until solution again, at last at 120 ℃ of following drying treatment 24h of vacuum drying oven.
(2) get above-mentioned carbon nanotube 0.5g and be dispersed in the 200ml water, add 0.5g anionic (SDS) again, sonic oscillation 2h behind the mechanical stirring 30min obtains dispersed good carbon nano tube suspension.
(3) be mixed with suspension after 150g acrylic anodic electrophoretic coating and 150ml deionization are mixed, induction stirring 12h behind (25 ℃) sonic oscillation 1h at room temperature obtains the acrylic anodic electrophoretic coating suspension of slaking.
(4) electrophoresis suspensioning liquid in the carbon nano tube suspension described in (2) and (3) is mixed, at 28 ℃ of following thermostatic ultrasonic vibration 60min.
(5) insert two electrodes respectively as anode and negative electrode at the electrophoresis suspensioning liquid described in (4), anode and negative electrode are respectively stainless steel plate; Electrophoretic deposition under DC mode, keeping two interelectrode distances is that 1cm, electrophoretic voltage are that 50V, electrophoresis time are 120s, treat electrophoresis finish after in deionized water residual electrophoresis suspensioning liquid on the flush away electrode.
(6) carbon nanotube/vinylformic acid matrix material with electrophoretic deposition is drying 1h naturally in air, and 160 ℃ of curing 90min in vacuum drying oven promptly obtain final carbon nanotube/vinylformic acid matrix material again.
(7) in prepared carbon nanotube/vinylformic acid matrix material, content of carbon nanotubes is about 0.2%, and vinylformic acid accounts for 99.8%, and salt-fog resistant time is greater than 1000h, and acid resistance and alkali resistance all reach more than the 24h, and corrosion resistance nature is preferably arranged.
(1) takes by weighing the 1g carbon nanofiber, in ball mill with the rotating speed ball milling 2h of 4000rpm, then carbon nanofiber behind the ball milling is dispersed in the mixed acid solution of the 500ml vitriol oil/concentrated nitric acid (volume ratio is 4: 1), and at 120 ℃ of following reflow treatment 1h, be neutral with a large amount of deionized water wash until solution again, at last 80 ℃ of following drying treatment 24h in vacuum drying oven.
(2) get above-mentioned carbon nanofiber 0.5g and be dispersed in the 400ml water, add 1g aniorfic surfactant Sodium dodecylbenzene sulfonate (SDBS) again, sonic oscillation 0.5h behind the mechanical stirring 5min obtains dispersed good carbon nanofiber suspension.
(3) will be mixed with suspension after ester modified Resins, epoxy anode electrophoresis dope of 50g soft polyurethane and the mixing of 200ml deionization, induction stirring 24h behind (25 ℃) sonic oscillation 2h at room temperature obtains the ester modified Resins, epoxy anode electrophoresis dope of the soft polyurethane suspension of slaking.
(4) electrophoresis suspensioning liquid in the carbon nanofiber suspension described in (2) and (3) is mixed, at 34 ℃ of following thermostatic ultrasonic vibration 60min.
(5) insert two electrodes respectively as anode and negative electrode in the electrophoresis suspensioning liquid described in (4), anode and negative electrode are stainless steel plate; Electrophoretic deposition under DC mode, keeping two interelectrode distances is that 2cm, electrophoretic voltage are that 80V, electrophoresis time are 300s, treat electrophoresis finish after in deionized water residual electrophoresis suspensioning liquid on the flush away electrode.
(6) the ester modified epoxy resin composite material of the carbon nanofiber/soft polyurethane of electrophoretic deposition is being dried 2h naturally in air, 200 ℃ of curing 30min in vacuum drying oven promptly obtain the ester modified epoxy resin composite material of carbon nanofiber/soft polyurethane again.
(7) in the prepared ester modified epoxy resin composite material of carbon nanofiber/soft polyurethane, the carbon nanofiber massfraction is about 0.4%, the ester modified Resins, epoxy of soft polyurethane accounts for 99.6%, salt-fog resistant time is greater than 1100h, acid resistance and alkali resistance all reach more than the 24h, and corrosion resistance nature is preferably arranged.
Claims (8)
1. preparation method based on the electrophoretic deposition nano-polymer composite material, it is characterized in that, by with carbon nanotube or carbon nanofiber with add water after tensio-active agent mixes and obtain carbon nanometer electrophoresis suspensioning liquid, then with maturation process after anode electrophoresis dope or cathode electrophoresis dope mixes after electrophoretic deposition and solidification treatment obtain nano-polymer composite material;
Described electrophoretic deposition is meant: electrophoretic voltage 40-200V, interelectrode distance 1-10cm, electrophoretic deposition time 30-300s, electrophoresis suspensioning liquid temperature are 25-35 ℃ under DC mode and constant voltage, and the effect of electric field lower surface has the carbon nanotube of like charges or carbon nanofiber and polymer molecule together to the opposite electrode swimming of charge property outside.
2. the preparation method based on the electrophoretic deposition nano-polymer composite material according to claim 1, it is characterized in that, described carbon nanotube or carbon nanofiber are cut through too short, purifying is modified and is handled, specifically be meant: with ball mill to carbon nanotube or carbon nanofiber to carrying out ball-milling processing, ball milling speed 100-6000rpm, ball milling time-300min, be 1 in volume ratio then: 9-9: in 1 the vitriol oil and the mixed acid solution of concentrated nitric acid 50-120 ℃ following reflow treatment 1-12 hour, postcooling to the room temperature of finishing dealing with is neutral with a large amount of deionized water wash until solution.
3. the preparation method based on the electrophoretic deposition nano-polymer composite material according to claim 2 is characterized in that, the described vitriol oil and concentrated nitric acid are respectively massfractions greater than 70% sulphuric acid soln and massfraction greater than 65% salpeter solution.
4. the preparation method based on the electrophoretic deposition nano-polymer composite material according to claim 1 is characterized in that, described tensio-active agent is cats product, anion surfactant or nonionogenic tenside.
5. the preparation method based on the electrophoretic deposition nano-polymer composite material according to claim 1, it is characterized in that, described maturation process is meant mixes anode electrophoresis dope or cathode electrophoresis dope and water by mass ratio 0.2-5, again through sonic oscillation and the polymer coating electrophoresis suspensioning liquid that obtains more than the mechanical stirring 12h.
6. the preparation method based on the electrophoretic deposition nano-polymer composite material according to claim 1 is characterized in that, the mass ratio of described carbon nanometer electrophoresis suspensioning liquid and anode electrophoresis dope or cathode electrophoresis dope is 0.2-5.
7. the preparation method based on the electrophoretic deposition nano-polymer composite material according to claim 1 is characterized in that, described solidification treatment is meant: toast 30-120min under 120-200 ℃ of environment.
8. one kind based on the electrophoretic deposition nano-polymer composite material, it is characterized in that, prepares according to the described method of above-mentioned arbitrary claim.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102409384A (en) * | 2011-11-04 | 2012-04-11 | 无锡中科光远生物材料有限公司 | Method for purifying colloid nanoparticles by using electrophoretic deposition |
| CN102605407A (en) * | 2012-03-05 | 2012-07-25 | 史建明 | Hole sealing method for aluminum and aluminium alloy anode oxide film |
| CN104711654A (en) * | 2015-03-18 | 2015-06-17 | 上海交通大学 | Graphene oxide/electrophoretic paint composite coating and method for preparing composite coating through electrophoretic deposition |
| CN105907367A (en) * | 2016-04-26 | 2016-08-31 | 中国科学院微电子研究所 | Preparation method of wave-absorbing material and wave-absorbing material prepared therefrom |
| WO2017024444A1 (en) * | 2015-08-07 | 2017-02-16 | Hewlett-Packard Development Company, L.P. | Coating conductive components |
| CN108796586A (en) * | 2018-06-25 | 2018-11-13 | 福州大学 | A kind of 3D printing method for the engraved structure orienting electrophoretic deposition based on light |
| CN108905924A (en) * | 2018-07-23 | 2018-11-30 | 东北大学秦皇岛分校 | A kind of chemical reaction equipment of controllable nano materials synthesis |
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Cited By (13)
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| CN102409384A (en) * | 2011-11-04 | 2012-04-11 | 无锡中科光远生物材料有限公司 | Method for purifying colloid nanoparticles by using electrophoretic deposition |
| CN102605407A (en) * | 2012-03-05 | 2012-07-25 | 史建明 | Hole sealing method for aluminum and aluminium alloy anode oxide film |
| CN104711654A (en) * | 2015-03-18 | 2015-06-17 | 上海交通大学 | Graphene oxide/electrophoretic paint composite coating and method for preparing composite coating through electrophoretic deposition |
| CN104711654B (en) * | 2015-03-18 | 2017-07-11 | 上海交通大学 | Graphene oxide/electrophoretic paint composite coating and its electrophoretic deposition preparation method |
| WO2017024444A1 (en) * | 2015-08-07 | 2017-02-16 | Hewlett-Packard Development Company, L.P. | Coating conductive components |
| CN105907367A (en) * | 2016-04-26 | 2016-08-31 | 中国科学院微电子研究所 | Preparation method of wave-absorbing material and wave-absorbing material prepared therefrom |
| CN108796586A (en) * | 2018-06-25 | 2018-11-13 | 福州大学 | A kind of 3D printing method for the engraved structure orienting electrophoretic deposition based on light |
| CN108796586B (en) * | 2018-06-25 | 2019-06-11 | 福州大学 | A kind of 3D printing method of the engraved structure based on light orientation electrophoretic deposition |
| CN108905924A (en) * | 2018-07-23 | 2018-11-30 | 东北大学秦皇岛分校 | A kind of chemical reaction equipment of controllable nano materials synthesis |
| CN113845756A (en) * | 2021-11-04 | 2021-12-28 | 西南石油大学 | Preparation method of basalt fiber composite material |
| CN113845756B (en) * | 2021-11-04 | 2023-09-05 | 西南石油大学 | Preparation method of basalt fiber composite material |
| CN114905674A (en) * | 2022-06-02 | 2022-08-16 | 西南石油大学 | Method for preparing aramid nano-fiber film through in-situ electrodeposition |
| CN114905674B (en) * | 2022-06-02 | 2023-09-01 | 西南石油大学 | Method for preparing aramid nanofiber film by in-situ electrodeposition |
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Application publication date: 20110914 |