CN104211962A - High dielectric polyimide composite material and preparation method thereof - Google Patents
High dielectric polyimide composite material and preparation method thereof Download PDFInfo
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- CN104211962A CN104211962A CN201410459609.5A CN201410459609A CN104211962A CN 104211962 A CN104211962 A CN 104211962A CN 201410459609 A CN201410459609 A CN 201410459609A CN 104211962 A CN104211962 A CN 104211962A
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Abstract
The invention relates to a polyimide nano composite material with a high dielectric constant and a preparation method thereof, and belongs to the field of organic/inorganic hybrid materials. The polyimide nano composite film material disclosed by the invention takes polyimide which is obtained by an anhydride monomer and a diamine monomer in a manner of polycondensation as the matrix and is doped with graphene and nano barium titanate, wherein the volume fraction of the graphene in the material is 0-3%; the volume fraction of nano barium titanate in the material is 0-20%; and the molar ratio of the anhydride monomer to the diamine monomer is (1.1 to 1) to 1. The polyimide nano composite material disclosed by the invention has a high dielectric constant and low loss, and can still keep good mechanical property, thereby overcoming the problems that an existing dual-phase high dielectric material is poor in tenacity, and difficult in control on packing amount and the like. The polyimide nano composite film material disclosed by the invention is suitable for components in microelectronic fields such as high-performance embedded capacitors, printed circuit boards and the like.
Description
Technical field
The invention belongs to organic/inorganic hybridization material field, be specifically related to a kind of have high-k and the lower polyimide nano composite thin film material of loss and preparation method thereof.
Background technology
Along with the development in electronics science field, thereby the research trend of electron device is realized the application in high power capacitor, embedded capacitor in miniaturization, high efficiency.Meanwhile, in some sensors, high frequency telecommunication equipment, the requirement of the high dielectric constant film material of demand also improves gradually.At present, in the electron device such as electrical condenser, conventional high dielectric constant film material mostly is inorganic ceramic material or polymer/inorganic composite film material.Although wherein inorganic ceramic material has higher specific inductivity, its machine-shaping temperature is up to more than 700 DEG C, and complex process; Although and polymer/inorganic composite film material has some improvement in mechanical property with respect to inorganic ceramic material, its film snappiness is still poor.There are reports in patent for this matrix material, all discloses a kind of high dielectric polymer/inorganic composite materials and point out its preparation method in patent CN101955667A, CN102875827A.Simultaneously, adulterate in the polyimide matrix CaCu 3 Ti 4 O of volume fraction 40% of the people such as the Dang Zhimin of University of Science & Technology, Beijing, under room temperature 100Hz condition, the specific inductivity of film can reach 49, and dielectric loss is less than 0.2 (Advanced Calcium Copper Titanate Polyimide Functional hybrid films with high dielectric permittivity, Advanced Material[J] 2009,21,2077 – 2082).Although overcome large, the unmanageable shortcoming of simple inorganic materials fragility, along with the increase of CaCu 3 Ti 4 O content, the mechanical property of film can significantly decrease, make the specific inductivity of material to reach bigger numerical by doped titanic acid copper calcium.
Meanwhile, another kind of high dielectric material polymkeric substance/conductive filler material laminated film is widely studied.The advantage of this material is, conductive filler material (as silver, carbon fiber, carbon nanotube etc.) wherein in doping hour, just can make the specific inductivity of film be significantly improved.For example, the quick result of study that waits people of party of University of Science & Technology, Beijing intelligence shows, in polyvinylidene difluoride (PVDF), when carbon fiber content reaches volume fraction 7.4%, the specific inductivity of composite film material can reach 80 (Dielectric properties of upright carbon fiber filled poly (vinylidene fluoride) composite with low percolation threshold and weak temperature dependence in the time of room temperature 100Hz, Applied Physics Letters[J] 2007,91,072912).But can there is violent variation in the time that the conductive particle of doping approaches percolation threshold in the specific inductivity of this matrix material, make the addition of conductive filler material be difficult to control, the best dielectric constant values of gained film is also difficult to repeat experiment.
Patent CN103275488A has introduced and used Graphene and nano barium phthalate after Ursol D graft modification is filler, compound with polyimide.Although wherein after conductive doped/mineral filler, the purer polyimide of specific inductivity of gained matrix material increases, but because its graft modification on Graphene has affected the conductivity that Graphene plays a major role, thereby limit the raising of this three-phase composite thin-film dielectric performance.
Summary of the invention
The object of the invention is to solve the deficiency in polymer composites performance in prior art, and provide one to prepare high dielectric composite polyimide material and preparation method thereof.
The polyimide that high dielectric composite polyimide material provided by the invention obtains taking dicarboxylic anhydride monomer and diamine monomer polycondensation is as matrix, and doped graphene and nano barium phthalate.Wherein the volume fraction of Graphene in material is 0～3%, and the volume fraction of nano barium phthalate in material is 0～20%.
Dicarboxylic anhydride monomer of the present invention comprises hexafluorodianhydride, diphenyl ether tetraformic dianhydride, pyromellitic acid anhydride, bibenzene tetracarboxylic dianhydride, according to complexity and the optimized film performance of preparation, further preferred hexafluorodianhydride and diphenyl ether tetraformic dianhydride.
Diamine monomer of the present invention comprises 4 ' 4-diaminodiphenyl oxide, Ursol D, according to complexity, cost consideration and the optimized film performance of preparation, further preferably 4 ' 4-diaminodiphenyl oxide, Ursol D.
Organic solvent of the present invention is N ' N-N,N-DIMETHYLACETAMIDE, N ' dinethylformamide, according to complexity, cost consideration and the optimized film performance of preparation, and further preferred N ' N-N,N-DIMETHYLACETAMIDE.
The molar ratio of dicarboxylic anhydride monomer of the present invention and diamine monomer is 1.1～1:1,
The method of high-k provided by the present invention and low-loss polyimide/graphene composite film is as follows:
1) Graphene is added in organic solvent, under room temperature, after ultrasonic dispersion 4～12h, add diamine monomer.Stir 10～30min, after diamine monomer all dissolves, under ice bath agitation condition, repeatedly add on a small quantity dicarboxylic anhydride monomer, after having fed in raw material, obtain the polyamic acid/graphene solution of certain viscosity.
2) polyamic acid/graphene solution obtaining is coated with out on smooth sheet material to the film of even thickness; Treat totally imidization 2～6h under 135～300 DEG C of environment of solvent evaporates, thereby obtain composite polyimide material.
The method of high-k provided by the present invention and low-loss polyimide/Graphene/barium titanate laminated film is as follows:
1) Graphene and barium titanate are added in organic solvent, under room temperature, after ultrasonic dispersion 4～12h, add diamine monomer.Stir 10～30min, after diamine monomer all dissolves, under ice bath agitation condition, repeatedly add on a small quantity dicarboxylic anhydride monomer, after having fed in raw material, obtain polyamic acid/Graphene/barium titanate solution of certain viscosity.
2) polyamic acid/Graphene obtaining/barium titanate solution is coated with out on smooth sheet material to the film of even thickness; Treat totally imidization 2～6h under 135～300 DEG C of environment of solvent evaporates, thereby obtain composite polyimide material.
Above-mentioned two steps 2) in use sheet material comprise stainless steel plate, silicon chip, the smooth surfaces such as sheet glass are smooth and have the planar materials of certain mechanical property and resistance toheat, are conducive to polyamic acid/Graphene or polyamic acid/Graphene/barium titanate and after moulding imidization, separate in the plane.
Ultrasonic dispersion in above-mentioned steps refers to that will be difficult to homodisperse Graphene and barium titanate particles in organic solvent with conventional ultrasonic method disperses.Therefore frequency and power for ultrasonic device do not have particular requirement, but due to the efficiency difference of each ultrasonic device, for the consideration to dispersion effect, ultrasonic time of the present invention is decided to be 4～12h.
Polyimide composite film material provided by the invention has the good mechanical property of polyimide material itself, has very high specific inductivity (>100) simultaneously under room temperature 100Hz condition.So the composite polyimide material obtaining according to method provided by the invention can be applied to ultracapacitor, sensor high-tech electronics field.
The present invention has following excellent effect:
High dielectric polyimide composite film provided by the present invention has excellent dielectric properties, and the introducing of mineral filler and conductive filler material does not destroy the mechanical property that polyimide matrix is good.In the time that Graphene massfraction reaches 2.5%, the specific inductivity of polyimide/graphene composite film material can reach 69 under room temperature 100Hz, is 21 times of pure Kapton.Meanwhile, in polyimide/Graphene provided by the invention/barium titanate laminated film, Graphene volume fraction is 1%, and when barium titanate volume fraction 15%, the specific inductivity of matrix material can reach more than 160, and its dielectric loss value remains on below 1.High dielectric composite polyimide material provided by the invention and preparation method thereof, the film that has not only overcome simple doping inorganic ceramic filler is along with filler content increases gradually and the serious phenomenon reducing of mechanical property occurs, and the specific inductivity that has overcome polymkeric substance/conductive filler material matrix material, in the time that the conductive particle of doping approaches percolation threshold, violent variation occurs, make the unmanageable defect of addition of conductive filler material.
Brief description of the drawings
Profile scanning electron microscope (SEM) photo of the polyimide/graphene composite film of preparation in Fig. 1, embodiment 1 (a) and embodiment 2 (b).
The section SEM photo of polyimide/Graphene/barium titanate laminated film of preparation in Fig. 2, embodiment 4 (a) and embodiment 5 (b).
Polyimide/graphene composite film specific inductivity of preparation and the variation relation of frequency in Fig. 3, embodiment 1,2,3,4 and comparative example 1.
Polyimide/Graphene/barium titanate laminated film mechanical property of preparation in Fig. 4, embodiment 5,6,7.
Embodiment
Below in conjunction with example, the present invention is further described.
1. the preparation of polyimide/graphene composite film:
Embodiment 1
1) 0.0166g Graphene and 10mlDMAc are joined in there-necked flask, after sealing, ultrasonic dispersion 8h.Under agitation condition, add 0.5067gODA, after it dissolves completely, add ice bath.Continue to stir, point 6 every 10min add 1.1367g6FDA altogether.20min is reacted in the rear continuation of having fed in raw material, and obtains polyamic acid/graphene solution;
2) polyamic acid/graphene solution is coated with out on sheet glass to the film of even thickness, at 135 DEG C and 300 DEG C imidization 1h and 2h respectively, obtains the polyimide composite film of Graphene volume fraction 0.63% (massfraction 1%).
Gained polyimide composite film is determined to 1 × 1cm print, utilize ion sputtering instrument to carry out dielectric properties test after the metal spraying of print two sides, result shows that the specific inductivity of this film composite material under room temperature 100Hz condition is 5.07, and dielectric loss is 1.7 × 10
-2.
Embodiment 2
1) 0.0332g Graphene and 10mlDMAc are joined in there-necked flask, after sealing, ultrasonic dispersion 8h.Under agitation condition, add 0.5016gODA, after it dissolves completely, add ice bath.Continue to stir, point 6 every 10min add 1.1252g6FDA altogether.20min is reacted in the rear continuation of having fed in raw material, and obtains polyamic acid/graphene solution;
2) polyamic acid/graphene solution is coated with out on sheet glass to the film of even thickness, at 135 DEG C and 300 DEG C imidization 1h and 2h respectively, obtains the polyimide composite film of Graphene volume fraction 1.26% (massfraction 2%).
Gained polyimide composite film is determined to 1 × 1cm print, utilize ion sputtering instrument to carry out dielectric properties test after the metal spraying of print two sides, result shows that the specific inductivity of this film composite material under room temperature 100Hz condition is 16.28, and dielectric loss is 3.1 × 10
-1.
Embodiment 3
1) 0.0382g Graphene and 10mlDMAc are joined in there-necked flask, after sealing, ultrasonic dispersion 8h.Under agitation condition, add 0.5000gODA, after it dissolves completely, add ice bath.Continue to stir, point 6 every 10min add 1.1218g6FDA altogether.20min is reacted in the rear continuation of having fed in raw material, and obtains polyamic acid/graphene solution;
2) polyamic acid/graphene solution is coated with out on sheet glass to the film of even thickness, at 135 DEG C and 300 DEG C imidization 1h and 2h respectively, obtains the polyimide composite film of Graphene volume fraction 1.45% (massfraction 2.3%).
Gained polyimide composite film is determined to 1 × 1cm print, utilize ion sputtering instrument to carry out dielectric properties test after the metal spraying of print two sides, result shows that the specific inductivity of this film composite material under room temperature 100Hz condition is 37.52, and dielectric loss is 1.35.
Embodiment 4
1) 0.0415g Graphene and 10mlDMAc are joined in there-necked flask, after sealing, ultrasonic dispersion 8h.Under agitation condition, add 0.499gODA, after it dissolves completely, add ice bath.Continue to stir, point 6 every 10min add 1.1195g6FDA altogether.20min is reacted in the rear continuation of having fed in raw material, and obtains polyamic acid/graphene solution;
2) polyamic acid/graphene solution is coated with out on sheet glass to the film of even thickness, at 135 DEG C and 300 DEG C imidization 1h and 2h respectively, obtains the polyimide composite film of Graphene volume fraction 1.58% (massfraction 2.5%).
Gained polyimide composite film is determined to 1 × 1cm print, utilize ion sputtering instrument to carry out dielectric properties test after the metal spraying of print two sides, result shows that the specific inductivity of this film composite material under room temperature 100Hz condition is 68, and dielectric loss is 8.9.
Comparative example 1
1) 0.512gODA and 10mlDMAc are joined in there-necked flask, after stirring is dissolved ODA completely, add ice bath.Continue to stir, point 6 every 10min add 1.149g6FDA altogether.20min is reacted in the rear continuation of having fed in raw material, and obtains polyamic acid solution;
2) polyamic acid solution is coated with out on sheet glass to the film of even thickness, at 135 DEG C and 300 DEG C imidization 1h and 2h respectively, obtains pure Kapton.
Gained Kapton is determined to 1 × 1cm print, utilize ion sputtering instrument to carry out dielectric properties test after the metal spraying of print two sides, result shows that the specific inductivity of this thin-film material under room temperature 100Hz condition is 3.44, and dielectric loss is 7.14 × 10
-3.Its dielectric loss value is starkly lower than polyimide/graphene composite film material.
2. the preparation of polyimide/Graphene/barium titanate laminated film:
Embodiment 5
1) 0.0061g Graphene, 1.4094g barium titanate and 15mlDMAc are joined in there-necked flask, after sealing, ultrasonic dispersion 8h.Under agitation condition, add 0.75gODA, after it dissolves completely, add ice bath.Continue to stir, point 6 every 10min add 1.1742gODPA altogether.20min is reacted in the rear continuation of having fed in raw material, and obtains polyamic acid/graphene solution;
2) polyamic acid/Graphene/barium titanate solution is coated with out on sheet glass to the film of even thickness, at 135 DEG C and 300 DEG C imidization 1h and 2h respectively, obtains Graphene volume fraction 0.2%, the polyimide composite film of barium titanate volume fraction 15%.
Gained polyimide composite film is determined to 1 × 1cm print, utilize ion sputtering instrument to carry out dielectric properties test after the metal spraying of print two sides, result shows that the specific inductivity of this film composite material under room temperature 100Hz condition is 8.01, and dielectric loss is 1.45 × 10
-2.
Embodiment 6
1) 0.02454g Graphene, 1.4094g barium titanate and 8mlDMAc are joined in there-necked flask, after sealing, ultrasonic dispersion 8h.Under agitation condition, add 0.6441gODA, after it dissolves completely, add ice bath.Continue to stir, point 6 every 10min add 1.009gODPA altogether.20min is reacted in the rear continuation of having fed in raw material, and obtains polyamic acid/graphene solution;
2) polyamic acid/Graphene/barium titanate solution is coated with out on sheet glass to the film of even thickness, at 135 DEG C and 300 DEG C imidization 1h and 2h respectively, obtains Graphene volume fraction 0.8%, the polyimide composite film of barium titanate volume fraction 15%.
Gained polyimide composite film is determined to 1 × 1cm print, utilize ion sputtering instrument to carry out dielectric properties test after the metal spraying of print two sides, result shows that the specific inductivity of this film composite material under room temperature 100Hz condition is 9.28, and dielectric loss is 8.75 × 10
-3.
Embodiment 7
1) 0.03075g Graphene, 1.4094g barium titanate and 15mlDMAc are joined in there-necked flask, after sealing, ultrasonic dispersion 8h.Under agitation condition, add 0.75gODA, after it dissolves completely, add ice bath.Continue to stir, point 6 every 10min add 1.1742gODPA altogether.20min is reacted in the rear continuation of having fed in raw material, and obtains polyamic acid/graphene solution;
2) polyamic acid/Graphene/barium titanate solution is coated with out on sheet glass to the film of even thickness, at 135 DEG C and 300 DEG C imidization 1h and 2h respectively, obtains Graphene volume fraction 1%, the polyimide composite film of barium titanate volume fraction 15%.
Gained polyimide composite film is determined to 1 × 1cm print, utilize ion sputtering instrument to carry out dielectric properties test after the metal spraying of print two sides, result shows that the specific inductivity of this film composite material under room temperature 100Hz condition is 164.09, and dielectric loss is 0.96.The specific inductivity of this laminated film is at filler addition hour just considerably beyond pure Kapton, and visible high dielectric composite polyimide material provided by the invention is as the superiority of dielectric materials.
By by the contrast of concrete test data in embodiment and comparative example, can prove, the specific inductivity of composite polyimide material provided by the invention is significantly improved than general polymer material, and after interpolation conductive filler material and inorganic ceramic filler, has still kept to a certain extent the mechanical property of polymkeric substance excellence.While moving closer to percolation threshold along with the content of conductive filler material Graphene, the specific inductivity of laminated film significantly improves, but simultaneously its dielectric loss also raises to some extent, until receptible maximum loss value in application process, obtain the maximum dielectric constant of laminated film.
Claims (6)
1. high dielectric composite polyimide material and preparation method thereof, it is characterized in that: the polyimide obtaining taking dicarboxylic anhydride monomer and diamine monomer polycondensation is as matrix, and doped graphene and nano barium phthalate, wherein the volume fraction of Graphene in material is 0～3%, the volume fraction of nano barium phthalate in material is 0～20%, and the molar ratio of dicarboxylic anhydride monomer and diamine monomer is 1.1～1:1.
2. high dielectric composite polyimide material of one according to claim 1 and preparation method thereof, it is characterized in that Graphene and barium titanate are dispersed in polyimide matrix, the lamellar spacing of Graphene is 0.335～1.2nm, lamella diameter is 0.5～5 μ m, and the diameter <100nm of nano barium titanate titanate particle.
3. high dielectric composite polyimide material of one according to claim 1 and preparation method thereof, is characterized in that described dicarboxylic anhydride monomer is hexafluorodianhydride, diphenyl ether tetraformic dianhydride, pyromellitic acid anhydride, bibenzene tetracarboxylic dianhydride.
4. high dielectric composite polyimide material of one according to claim 1 and preparation method thereof, is characterized in that described diamine monomer is 4 ' 4-diaminodiphenyl oxide, Ursol D.
5. high dielectric composite polyimide material and preparation method thereof, is characterized in that comprising the following steps:
(1) Graphene and barium titanate or Graphene are dispersed in organic solvent, through ultrasonic dispersion 4～12h under room temperature, it are fully disperseed and form Graphene/barium titanate or the uniform dispersion of Graphene in organic solvent;
(2) diamine monomer is added in Graphene/barium titanate or graphene dispersing solution, stirs 10～30min, after diamine monomer dissolves completely, under ice bath agitation condition, a small amount of repeatedly add dicarboxylic anhydride monomer; After having fed in raw material, obtain polyamic acid/Graphene/barium titanate or the polyamic acid/graphene solution of certain viscosity;
(3) polyamic acid/Graphene/barium titanate obtaining or polyamic acid/graphene solution are coated with out to the film of even thickness at smooth plate surface; Treat solvent evaporates totally, imidization 2～6h under 135～300 DEG C of environment, thus obtain polyimide composite film material.
6. according to the method for the synthetic high-k described in right 5 and low-loss polyimide/Graphene/barium titanate laminated film, it is characterized in that described organic solvent is N ' N-N,N-DIMETHYLACETAMIDE, N ' dinethylformamide, described dicarboxylic anhydride monomer is hexafluorodianhydride, diphenyl ether tetraformic dianhydride, pyromellitic acid anhydride, bibenzene tetracarboxylic dianhydride, described diamine monomer is 4 ' 4-diaminodiphenyl oxide, Ursol D, and wherein the molar ratio of dicarboxylic anhydride monomer and diamine monomer is 1.1～1:1.
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| CN105038228A (en) * | 2015-08-03 | 2015-11-11 | 铜陵市胜达电子科技有限责任公司 | Polyimide high-dielectric composite film mixed with nano-boron carbide-loaded graphene and used for capacitor and preparation method thereof |
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| CN105061790A (en) * | 2015-08-03 | 2015-11-18 | 铜陵市胜达电子科技有限责任公司 | Nano-barium titanate blended and nano-cerium dioxide loaded polyimide high dielectric composite film for capacitors and preparation method thereof |
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| CN108203543A (en) * | 2016-12-16 | 2018-06-26 | 中国科学院宁波材料技术与工程研究所 | Graphene enhancing polyimide nano-composite material and preparation method and application |
| CN109575595A (en) * | 2017-09-29 | 2019-04-05 | 肖干凤 | A kind of preparation method of polyetherimide/barium titanate/graphene dielectric composite material |
| CN108359238A (en) * | 2018-02-28 | 2018-08-03 | 佛山慧创正元新材料科技有限公司 | The preparation method of high temperature resistant compound polyimide dielectric material |
| CN110279895A (en) * | 2019-06-28 | 2019-09-27 | 江西理工大学 | A kind of l-lactic acid composite material and preparation method of barium titanate and graphene oxide collaboration enhancing |
| CN110279895B (en) * | 2019-06-28 | 2022-03-11 | 江西理工大学 | Barium titanate and graphene oxide synergistically enhanced levorotatory polylactic acid composite material and preparation method thereof |
| CN111635631A (en) * | 2020-05-26 | 2020-09-08 | 广东德星聚合物薄膜材料研究有限公司 | Polyimide composite material with high dielectric constant and preparation method thereof |
| CN114410111A (en) * | 2022-01-26 | 2022-04-29 | 四川轻化工大学 | Method for improving dielectric constant of composite film by graphitized multi-walled carbon nano-tube |
| CN114559721A (en) * | 2022-03-04 | 2022-05-31 | 西南科技大学 | Sandwich-structure high-energy-storage-density polyimide-based composite film and preparation method thereof |
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