CN102337019A - Polyaryletherketone/polyaniline-carbon nanotube composite material with high dielectric property and preparation method thereof - Google Patents
Polyaryletherketone/polyaniline-carbon nanotube composite material with high dielectric property and preparation method thereof Download PDFInfo
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- CN102337019A CN102337019A CN2011102332900A CN201110233290A CN102337019A CN 102337019 A CN102337019 A CN 102337019A CN 2011102332900 A CN2011102332900 A CN 2011102332900A CN 201110233290 A CN201110233290 A CN 201110233290A CN 102337019 A CN102337019 A CN 102337019A
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Abstract
The invention relates to a polyaryletherketone/polyaniline-carbon nanotube composite material with a high dielectric property and a preparation method thereof, and belongs to the technical field of a polymer base nano composite material and a preparation method thereof. The composite material comprises the following components in percentage by weight: 10-50% of carbon nanotubes wrapped by polyaniline and the balance of sulfonated polyetheretherketone. In the preparation method, the polyaniline-carbon nanotubes are used as a modified filling material, the sulfonated polyetheretherketone is used as a matrix material, N-methyl pyrrolidone is used as a solvent, and the materials are blended uniformly into a solution which is then cast into a mold. In the invention, because the organic wrapping layer of the filling material not only can make particles dispersed uniformly, but also can reduce the possibility of the generation of seepage current, dielectric constants are ensured, and simultaneously the dielectric loss is reduced. The obtained high dielectric composite material with good processability and good dielectric property can be applied in embedded capacitors.
Description
Technical field
The invention belongs to the technical field of polymer based nanocomposites and preparation thereof, particularly have polyaryletherketone/polyaniline-carbon nano tube compound material of high dielectric property and preparation method thereof.
Background technology
The most important character of dielectric materials is can polarize under the External Electrical Field, and specific inductivity (ε) is the important indicator that characterizes a kind of dielectric materials performance.Fast development along with electronic industry; Have the high dielectric constant material of good blocking-up current carrier, energy storage electric energy and uniform electric field effect during the dynamic RAM of storer class, transmitter miscellaneous, electrical condenser, photoelectricity/electro-optical device, microwave, particularly aspect electric power capacitor, integrated chip type electrical condenser, the motor cable field very important use is being arranged.Therefore; High dielectric constant materials is very crucial for the store energy industry; Because the demand of electric energy often is a discontinuity or irregular, must carry out electrical power storage and control efficiently, will be and improve capacitor stores density through improving the effective dielectric constant of material.
Present most high dielectric material is to use ferroelectric material---mainly is that ferroelectric ceramic(s) is made,, therefore can not processes the respective element of very big area because the ferroelectric material processing temperature is high, cohesive force is poor each other.The polymkeric substance light weight, be prone to processing, have multiple dimensioned structure and special snappiness, be very suitable for the dielectric materials preparation, but the specific inductivity lower (ε＜10) of exhausted big number polymer materials.A Basic Ways that improves the polymer materials dielectric properties is exactly (like BaTiO with the ceramic packing with high-k
3) add in the polymer materials.Polymkeric substance/ferroelectric ceramic(s) matrix material is compared with general ferroelectric ceramic(s) high dielectric material, has extraordinary processing characteristics, lower processing temperature and dielectric loss, can prepare the bigger device of area and volume ratio, and cost is also low than ferroelectric material simultaneously.For making its specific inductivity reach the industrial application level; Must satisfy very high ceramic particle charge capacity (surpassing 50% usually) just can make the polymkeric substance specific inductivity improve more than 10 times; But can reduce significantly like this polymer materials itself mechanical property and cohesiveness, increase porosity, reduce its suitability as electronic material.In addition, a kind of effective dielectric materials also must have stable dielectric properties under life-time service process and differing temps environment, but the specific inductivity of some ferroelectric ceramic materials but has much relations with particle size and temperature
In order to satisfy the requirement that embeds capacitor material, people are devoted to the R and D of high dielectric material always.But, also do not obtain the dielectric materials that a kind of ideal can be used for embedded capacitor up to now.Existing material also has problems in some aspects, comprises electrical property, mechanical property, processing characteristics etc., but a lot of materials have potential very widely application.Matrix material of the present invention combines polymkeric substance excellent properties and good processing characteristics, and organic coating layer not only can increase the consistency of filler and polymeric matrix, makes the particle homodisperse; And can outside conducting particles, form coating layer; Reduce the possibility that the seepage flow electric current produces, when guaranteeing specific inductivity, reduce its dielectric loss; Obtain having the high-dielectric composite material of good dielectric properties, get a good chance of in embedded capacitance, obtaining to use.
Summary of the invention
The purpose of this invention is to provide a kind of polyaryletherketone/polyaniline-carbon nano tube compound material (that is, sulfonated polyether ketone and polyaniline coated carbon nanotube matrix material) and preparation method thereof with high dielectric property.Through the functional modification to poly aryl ether ketone polymer, and selection function sulfonic acid doped with polyaniline-carbon nanotube is as packing material, thereby obtains the polyaryletherketone/polyaniline-carbon nano tube compound material of high dielectric property.
The preparation method of polyaryletherketone/polyaniline-carbon nano tube compound material utilizes polyaniline-carbon nanotube as the modification packing material; The functional poly aryl ether ketone is that sulfonated polyether ketone is as body material; Through the method for solution blending, the functional poly aryl ether ketone/polyaniline-carbon nano tube compound material of preparation high dielectric property.
High dielectric property polyaryl ether ketone/polyaniline of the present invention-carbon nano tube compound material; Moity comprises sulfonated polyether ketone and polyaniline coated carbon nanotube; By massfraction be 100% to calculate, the polyaniline coated carbon nanotube accounts for 5～45%, and all the other are sulfonated polyether ketone.
Sulfonated polyether ketone copolymer, its structural formula is as follows:
Wherein x/y is 5/95～40/60, and preferred ratio is 20/85～30/70; The scope of sulfonated polyether ketone viscosity is 1.0～2.0 (with the DMAC N,N are solvent, and strength of solution is 0.5g/dL); The preparation process of sulfonated polyether ketone can (2005,255, the method for delivering in 149-155) be synthetic at Journal of Membrane Science. according to Xianfeng Li.
Polyaniline-carbon nanotube that the present invention adopts is the method that adopts in-situ polymerization; At carbon nano tube surface parcel polyaniline; Carbon nanotube (Chengdu organic chemistry institute; Diameter is 10～20nm, and length is 10～30 μ m) use carboxylic acid to handle, but the preparation process reference literature of polyaniline-carbon nanotube (J Mater Sci 200843:3664-3669) preparation.Wherein the input amount of aniline and carbon nanotube in molar ratio ratio can be 40/60～80/20.Be polyaniline-carbon nanotube, the mass ratio of aniline and carbon nanotube is 40: 60～80: 20.
The preparation method of functional poly aryl ether ketone/polyaniline of the present invention-carbon nano tube compound material; Be to be body material with the sulfonated polyether ketone; With the polyaniline coated carbon nanotube is packing material, and packing material is dispersed under ultrasonication in the N-Methyl pyrrolidone (NMP); Body material is dissolved in the N-Methyl pyrrolidone (NMP); Again two kinds of N-Methyl pyrrolidone solution are mixed and continue to stir homogenizing; Then mixing solutions is cast into mould,, under 110～130 ℃, vacuum tightness≤0.1MPa condition, dried by the fire 16～36 hours again, promptly obtain the functional poly aryl ether ketone/polyaniline-carbon nano tube compound material of high dielectric property 60～80 ℃ of oven dry; Wherein, by body material and packing material massfraction be 100% to calculate, the polyaniline coated carbon nanotube accounts for 5～45%, and the concentration of the N-Methyl pyrrolidone solution of packing material is 0.005～0.1g/mL; The concentration of the N-Methyl pyrrolidone solution of body material is 0.05～0.3g/mL.
The above-mentioned mould that is cast into promptly can be mixing solutions to be poured on form liquid film on the flat glass plate naturally, and the oven dry back forms solid-state thin-film material; Also can cast in the model (tool) or container of Any shape, be formed with the goods of certain thickness solid shape after the oven dry.That is, the described mould that is cast into is mixing solutions to be poured on form liquid film on the flat glass plate naturally, and the oven dry back forms solid-state thin-film material; Or cast in model, mould or the container, the oven dry back forms the goods of solid shape.
Traditional ferroelectrics is generally inorganic materials; Ferroelectrics/polymer composites will reach very high specific inductivity; The loading level of general ferroelectric ceramic(s) will be very high, makes that the dielectric loss of matrix material is very high, and too high loading level will cause processing characteristics to descend.The present invention selects for use sulfonated polyether ketone as body material, and polyaniline-carbon nanotube is combined into high dielectric property polyaryl ether ketone/polyaniline-carbon nano tube compound material as packing material.Because organic coating layer of packing material not only can increase the consistency of filler and polymeric matrix; Make the particle homodisperse, and can outside conducting particles, form coating layer, reduce the possibility that the seepage flow electric current produces; When guaranteeing specific inductivity, reduce its dielectric loss; And matrix material has kept good processing characteristics of polymkeric substance and lower processing temperature.By the high-dielectric composite material that the present invention obtains, can in embedded capacitance, obtain to use with excellent machinability and good dielectric properties.
Description of drawings
Fig. 1 is the TEM photo (being used for comparing with Fig. 2) of carbon nanotube.
Fig. 2 is the (aniline: the TEM photo of packing material carbon nanotube=8: 2) of polyaniline-carbon nanotube among the embodiment of the invention 1-5.With respect to the obviously rough and chap of change of pure nano-carbon tube.
Fig. 3 is the SEM photo of the high dielectric property polyaryl ether ketone/polyaniline-carbon nano tube compound material of preparation in the embodiment of the invention 3.
Dark-coloured part is a polymeric matrix among the figure, and white bright spot is polyaniline-carbon nanotube, can see that polyaniline-carbon nanotube is uniformly dispersed in the polyaryletherketone matrix.
Embodiment
Following embodiment further specifies of the present invention, rather than limits scope of the present invention.
Embodiment 1:
With 0.1 gram polyaniline-carbon nanotube (aniline: carbon nanotube=8: 2, the material pattern is seen Fig. 2) in 2mlNMP ultrasonic 2 hours, make its homodisperse; Simultaneously 0.9 gram sulfonated polyether ketone (x/y=20/80) is dissolved among the 5ml NMP; Then two solution are mixed and continue to be cast on the level and smooth sheet glass after ultrasonic 1 hour, after 80 ℃ of oven dry, continued under 120 ℃ of temperature vacuum-drying 24 hours, promptly obtain high-k polyarylether ketone/carbon nanotube matrix material.
Measure the dielectric properties of material, its DIELECTRIC CONSTANTS=15, dielectric loss 0.11 (25 ℃ of probe temperatures, test frequency 1000Hz).
Embodiment 2:
With 0.2 gram polyaniline-carbon nanotube (aniline: carbon nanotube=8: 2, the material pattern is seen Fig. 2) in 4mlNMP ultrasonic 2 hours, make its homodisperse; Simultaneously 0.8 gram sulfonated polyether ketone (x/y=20/80) is dissolved among the 4ml NMP; Then two solution are mixed and continue to be cast on the level and smooth sheet glass after ultrasonic 1 hour, after 80 ℃ of oven dry, continued under 120 ℃ of temperature vacuum-drying 24 hours, make high-k polyarylether ketone/carbon nanotube matrix material.
Measure the dielectric properties of material, its DIELECTRIC CONSTANTS=159, dielectric loss 0.34 (25 ℃ of probe temperatures, test frequency 1000Hz).
Embodiment 3:
With 0.3 gram polyaniline-carbon nanotube (aniline: carbon nanotube=8: 2, the material pattern is seen Fig. 2) in 4mlNMP ultrasonic 2 hours, make its homodisperse; Simultaneously 0.7 gram sulfonated polyether ketone (x/y=20/80) is dissolved among the 5ml NMP; Then two solution are mixed and continue to be cast on the level and smooth sheet glass after ultrasonic 1 hour, after 70 ℃ of oven dry, continued under 130 ℃ of temperature vacuum-drying 16 hours.
The pattern of the high-k polyarylether ketone/carbon nanotube matrix material that makes is seen Fig. 3, measures the dielectric properties of material, DIELECTRIC CONSTANTS=1002, dielectric loss 3.19 (25 ℃ of probe temperatures, test frequency 1000Hz).
Choose sulfonated polyether-ether-ketone/carbon nanotube (mass ratio 94/6) matrix material reported and the material of this instance and do comparison; This matrix material content of carbon nanotubes also is 6%; Because do not have polyaniline to coat, carbon nanotube is not fine at the polymeric matrix dispersive, and the DIELECTRIC CONSTANTS of matrix material=480; Dielectric loss 120 (25 ℃ of probe temperatures, test frequency 1000Hz).The specific inductivity of this material is half the less than the specific inductivity of this patent material, and dielectric loss is 40 times of this patent material nearly.(Soft?Materials，2011，9：94-103)
Embodiment 4:
With 0.4 gram polyaniline-carbon nanotube (aniline: carbon nanotube=8: 2, the material pattern is seen Fig. 2) in 6mlNMP ultrasonic 2 hours, make its homodisperse; Simultaneously 0.6 gram sulfonated polyether ketone (x/y=20/80) is dissolved among the 3ml NMP; Then two solution are mixed and continue to be cast on the level and smooth sheet glass after ultrasonic 1 hour, after 80 ℃ of oven dry, continued under 120 ℃ of temperature vacuum-drying 24 hours, make high-k polyarylether ketone/carbon nanotube matrix material.
Measure the dielectric properties of material, DIELECTRIC CONSTANTS=1903, dielectric loss 9.97 (25 ℃ of probe temperatures, test frequency 1000Hz).
Embodiment 5:
Sulfonated polyether ketone among the embodiment 1 (x/y=20/80) is changed to sulfonated polyether ketone (x/y=30/70); With two solution mix continue to stir 12 hours (in embodiment 1～4, also can be without ultrasonic agitation, the churned mechanically time will be grown; Generally to stir 12～24 hours); Be cast to then on the level and smooth sheet glass, after 80 ℃ of oven dry, continue the following 130 ℃ of bakings of vacuum condition 24 hours.Can get high-k polyarylether ketone/carbon nanotube matrix material equally.
Embodiment 6:
With (the aniline: carbon nanotube=8: 2) be changed to aniline: the material of carbon nanotube=7: 3 or 6: 4 of polyaniline-carbon nanotube among embodiment 1～embodiment 4; All the other conditions are constant, still can obtain above-mentioned high-k polyarylether ketone/carbon nanotube matrix material.
Claims (5)
1. high dielectric property polyaryl ether ketone/polyaniline-carbon nano tube compound material; Moity is sulfonated polyether ketone and polyaniline coated carbon nanotube; By massfraction be 100% to calculate, the polyaniline coated carbon nanotube accounts for 5～45%, and all the other are sulfonated polyether ketone.
2. high dielectric property polyaryl ether ketone/polyaniline according to claim 1-carbon nano tube compound material is characterized in that, described sulfonated polyether ketone copolymer, and its structural formula is as follows:
Wherein x/y is 5/95～40/60; The scope of sulfonated polyether ketone viscosity is 1.0～2.0, is solvent with the DMAC N,N, and strength of solution is 0.5g/dL.
3. high dielectric property polyaryl ether ketone/polyaniline according to claim 1-carbon nano tube compound material is characterized in that, described polyaniline coated carbon nanotube, and the mass ratio of aniline and carbon nanotube is 40: 60～80: 20.
4. the preparation method of the high dielectric property polyaryl ether ketone/polyaniline of a claim 1-carbon nano tube compound material; Be to be body material with the sulfonated polyether ketone; With the polyaniline coated carbon nanotube is packing material, and packing material is dispersed in the N-Methyl pyrrolidone under ultrasonication; Body material is dissolved in the N-Methyl pyrrolidone; Again two kinds of N-Methyl pyrrolidone solution are mixed and continue to stir homogenizing; Then mixing solutions is cast into mould,, under 110～130 ℃, vacuum tightness≤0.1MPa condition, dried by the fire 16～36 hours again, obtain the functional poly aryl ether ketone/polyaniline-carbon nano tube compound material of high dielectric property 60～80 ℃ of oven dry; Wherein, the concentration of the N-Methyl pyrrolidone solution of packing material is 0.005～0.1g/mL; The concentration of the N-Methyl pyrrolidone solution of body material is 0.05～0.3g/mL.
5. the preparation method of high dielectric property polyaryl ether ketone/polyaniline according to claim 4-carbon nano tube compound material; It is characterized in that; The described mould that is cast into is mixing solutions to be poured on form liquid film on the flat glass plate naturally, and the oven dry back forms solid-state thin-film material; Or cast in model, mould or the container, the oven dry back forms the goods of solid shape.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104292452A (en) * | 2014-09-09 | 2015-01-21 | 天津师范大学 | Fluorenyl poly(ether-ether-ketone-ketone-ketone) thermoplastic resin and preparation method thereof |
| CN105524413A (en) * | 2015-11-03 | 2016-04-27 | 南京肯特复合材料有限公司 | Antistatic PEEK/PTFE composite material and preparation method thereof |
| CN105524412A (en) * | 2015-11-03 | 2016-04-27 | 南京肯特复合材料有限公司 | Antistatic peek resin material and preparation method thereof |
| CN107596932A (en) * | 2017-10-16 | 2018-01-19 | 黑龙江青谷酒庄有限公司 | A kind of cation-exchange membrane and its preparation method and application |
| US10866001B2 (en) | 2014-06-16 | 2020-12-15 | Core Energy Recovery Solutions Inc. | Blended membranes for water vapor transport and methods for preparing same |
| US11118053B2 (en) | 2018-03-09 | 2021-09-14 | Ticona Llc | Polyaryletherketone/polyarylene sulfide composition |
| US11352480B2 (en) | 2016-03-18 | 2022-06-07 | Ticona Llc | Polyaryletherketone composition |
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| CN1680457A (en) * | 2003-12-30 | 2005-10-12 | 吉林大学 | Sulfonated polyether ketone copolymer and its synthesis |
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| US10866001B2 (en) | 2014-06-16 | 2020-12-15 | Core Energy Recovery Solutions Inc. | Blended membranes for water vapor transport and methods for preparing same |
| CN104292452A (en) * | 2014-09-09 | 2015-01-21 | 天津师范大学 | Fluorenyl poly(ether-ether-ketone-ketone-ketone) thermoplastic resin and preparation method thereof |
| CN105524413A (en) * | 2015-11-03 | 2016-04-27 | 南京肯特复合材料有限公司 | Antistatic PEEK/PTFE composite material and preparation method thereof |
| CN105524412A (en) * | 2015-11-03 | 2016-04-27 | 南京肯特复合材料有限公司 | Antistatic peek resin material and preparation method thereof |
| US11352480B2 (en) | 2016-03-18 | 2022-06-07 | Ticona Llc | Polyaryletherketone composition |
| CN107596932A (en) * | 2017-10-16 | 2018-01-19 | 黑龙江青谷酒庄有限公司 | A kind of cation-exchange membrane and its preparation method and application |
| CN107596932B (en) * | 2017-10-16 | 2020-11-17 | 黑龙江青谷酒庄有限公司 | Cation exchange membrane and preparation method and application thereof |
| US11118053B2 (en) | 2018-03-09 | 2021-09-14 | Ticona Llc | Polyaryletherketone/polyarylene sulfide composition |
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