CN103013004A - Carbon/silicon core-shell structure-polymer high-dielectric composite material - Google Patents
Carbon/silicon core-shell structure-polymer high-dielectric composite material Download PDFInfo
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- CN103013004A CN103013004A CN2013100181271A CN201310018127A CN103013004A CN 103013004 A CN103013004 A CN 103013004A CN 2013100181271 A CN2013100181271 A CN 2013100181271A CN 201310018127 A CN201310018127 A CN 201310018127A CN 103013004 A CN103013004 A CN 103013004A
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Abstract
The invention provides a preparation method for carbon/silicon core-shell structure-polymer high-dielectric composite material which is excellent in dielectric performance. The preparation method includes: filling carbon in a silicon molecular sieve by a certain method to obtain a carbon/silicon core-shell structure material, and scattering the carbon/silicon core-shell structure material to prepare the composite material excellent in dielectric performance. Dielectric constant of the composite material can reach 2030, and dielectric loss is 2.02. The preparation method for the carbon/silicon core-shell structure-polymer high-dielectric composite material is simple in process, low in cost and free of pollution and is a promising method for preparing polymer-based dielectric composite materials.
Description
Technical field
The invention belongs to technical field of composite materials, relate to a kind of polymer-based carbon composite dielectric material that contains carbon/silicon nucleocapsid structure material.
Background technology
In recent years, polymer materials is because wide material sources, with low cost, excellent performance, free of contamination characteristics make it have a wide range of applications in the dielectric materials field, and more and more is subject to people's attention.Compare with the traditional ceramics dielectric materials, polymer materials has overcome that complete processing is complicated, cost is high, poor mechanical property, with serious pollution problem, but the specific inductivity of organic polymer material itself is lower, and this has just limited its application in the dielectric field.In order to obtain higher dielectric constant material, people attempt adding the high dielectric ceramic powder in polymkeric substance, but when ceramic addition reached a very large value, the toughness of matrix material can reduce.Current, it is found that when adding micro-nanometer conductive material in polymeric matrix, its dielectric properties have obtained greatly improving, and have kept again the good toughness of polymer materials simultaneously.
In nanometer conductive material, owing to nano-carbon material (carbon nanotube, carbon nano wire, carbon nano fiber, nano carbon microsphere, Graphene etc.) has excellent performance, the advantage such as with low cost gets more and more people's extensive concerning.Current, the key issue of a restriction preparation high dielectric property nano-sized carbon-polymer composites is exactly the agglomeration of nano-carbon material in polymer materials.For this reason, people attempt adopting chemical meteorology deposition (CVD) method to grow at silicon carbide and arrange carbon nanotube regular, that be evenly distributed, then with after the mixed with polymers prepare the polymer-based carbon dielectric materials (Appl.Phys.Lett.98 that the outstanding even carbon nanotube of dielectric properties distributes, 032901,2011).In addition, the carbon nanotube that it is found that chemically modified can be dispersed in the polymer materials, thereby, the formation of carbon nanotube conducting network and the increase of leakage current in the polymer materials have effectively been stoped, and then so that the dielectric properties of carbon nano tube-polymer matrix material are greatly improved (J.Phys.Chem.C113,17626-17629,2009).In recent years, people utilize the good solvent dispersion of graphene oxide to prepare the finely dispersed matrix material of graphene oxide, obtained again the graphene-polymer matrix material (Nano Lett.12,84,2012) of dielectric properties excellences by the method reduction of thermal reduction.In a word, improve content and the dispersiveness of nano-carbon material in polymer materials, prevent that it from forming the key that conductive network is preparation high dielectric property nano-sized carbon-polymer composites.
Therefore, we have chosen the SBA-15 si molecular sieves with two-dimentional hexagonal structure and inner duct arrangement homogeneous, adopt certain method to insert in carbon and obtain carbon/silicon nucleocapsid structure material in the molecular sieve pore passage, again it is mixed with polyvinylidene difluoride (PVDF) (PVDF) as filler and make polymer matrix composite, carbon is evenly dispersed in the polymer materials, and this material has excellent dielectric properties.In addition, the method is simple, and is with low cost, pollution-free, is fit to batch production, is a kind of method of promising making polymer-based carbon dielectric composite material.
Summary of the invention
The objective of the invention is by with carbon/silicon nucleocapsid structure dispersion of materials in polymkeric substance, prepare the matrix material with high dielectric property.
The below illustrates the implementation procedure of the object of the invention with specific examples, at first we adopt secondary dipping process, under the catalysis of sulfuric acid, sucrose solution is inserted in the duct of SBA-15, then, put into tube furnace after being dried and carry out high temperature carbonization, obtain take si molecular sieves as shell, the hud typed structured material of carbon is filled out in inside.This nucleocapsid structure material is by the obstruct of silicon, improved the dispersiveness of carbon material in polymkeric substance, the a large amount of reunions between the carbon material have effectively been avoided, stoped the formation of conductive network, thereby obviously improved the percolation threshold of polymer matrix composite, and then obtained the matrix material of high-k.
Utilize carbon/silicon nucleocapsid structure material and PVDF to prepare the concrete steps of high-performance dielectric composite material as follows:
(1) the 0.141 gram vitriol oil, 1.25 gram sucrose are dissolved in 5 ml waters, in this solution, add 1.00 gram SBA-15, ultra-sonic dispersion dipping 30 minutes.
(2) with the pasty mixture of gained 70 ℃ lower dry 1 hour, more respectively 100 ℃ and 160 ℃ of charings 6 hours.
(3) dark brown solid with gained grinds to form fine powder, repeats above-mentioned dipping and low-temperature carbonization process, and the quality of flooding for the second time impregnating solution useful is that primary 66%(keeps sucrose, and the mass ratio of sulfuric acid and water is identical when flooding first).
(4) the gained mixture is inserted in the tube furnace, under nitrogen protection, be warming up to 900 ℃ of charings 3 hours with the speed of 5 ℃ of per minutes.
(5) after the cooling, use deionized water wash, drying obtains carbon/silicon nucleocapsid structure material.
(6) take by weighing the carbon that a certain amount of process (1)-(5) step makes/silicon nucleocapsid structure material, after adding a certain amount of ethanol, ultra-sonic dispersion 3 hours, take by weighing afterwards a certain amount of PVDF powder, the gradation of PVDF powder is joined in carbon/silicon nucleocapsid structure material and the alcohol mixeding liquid, continued afterwards ultra-sonic dispersion 2 hours, the suspension liquid that obtains mixing.Suspension liquid is poured in the watch-glass, and 80 ℃ were descended dry 4 hours, dried material is ground in agate mortar obtain trickle powder.
(7) get the fine-powder that a certain amount of (6) step obtains, use powder compressing machine that its pressure is thin slice, then thin slice is placed 200 ℃ of lower insulations 3 hours, obtain carbon/silicon nucleocapsid structure-PVDF matrix material.With the slice surfaces polishing, the surface-coated conductive silver glue can carry out the measurement of electrical properties after the oven dry.
Can obtain the dielectric composite material that carbon/silicon nucleocapsid structure and PVDF are composited by said process, this material has higher specific inductivity and low dielectric loss, and relative permittivity can reach 2030, and this moment, dielectric loss was 2.02(1kHz).
The method for preparing the polymer-based carbon high-dielectric composite material provided by the present invention is by carbon/silicon nucleocapsid structure dispersion of materials is prepared high-dielectric composite material in polymkeric substance.Compare with more existing chemical modification methods, under identical specific inductivity, have less dielectric loss.The method is with low cost, and is simple, pollution-free, has great using value in nano-sized carbon-polymkeric substance composite dielectric material field.
Description of drawings
Fig. 1 is that (Fig. 1 a) disperses the schematic diagram of (Fig. 1 b) to carbon/silicon nucleocapsid structure material at the PVDF camber with it.
Fig. 2 is the carbon/silicon nucleocapsid structure material of different ratios and matrix material specific inductivity that PVDF is composited, and (Fig. 2 dielectric loss a) and under 1kHz changes the relation curve of (Fig. 2 b) with carbon/silicon nucleocapsid structure quality of materials mark with frequency change.
Embodiment
Describe the present invention in detail below in conjunction with drawings and Examples.
Embodiment 1, and the 0.141 gram vitriol oil, 1.25 gram sucrose are dissolved in 5 ml waters, adds 1.00 gram SBA-15, ultra-sonic dispersion dipping 30 minutes in this solution.With the pasty mixture of gained 70 ℃ lower dry 1 hour, more respectively 100 ℃ and 160 ℃ of charings 6 hours.The dark brown solid of gained is ground to form fine powder, repeat above-mentioned dipping and low-temperature carbonization process, the quality of flooding for the second time impregnating solution useful is that primary 66%(keeps sucrose, and the mass ratio of sulfuric acid and water is identical when flooding first).The gained mixture is inserted in the tube furnace, under nitrogen protection, be warming up to 900 ℃ of charings 3 hours with the speed of 5 ℃ of per minutes.After the cooling, use deionized water wash, drying obtains carbon/silicon nucleocapsid structure material, as shown in Figure 1a.
Take by weighing a certain amount of carbon/silicon nucleocapsid structure material, add an amount of ethanol after, ultra-sonic dispersion 3 hours, take by weighing afterwards a certain amount of PVDF powder, the gradation of PVDF powder is joined in silicon﹠amp and the alcohol mixeding liquid, continued afterwards ultra-sonic dispersion 2 hours, the suspension liquid that obtains mixing.Suspension liquid is poured in the watch-glass, and 80 ℃ were descended dry 4 hours, and dried material is ground in agate mortar, obtained trickle powder.
Get a certain amount of above-mentioned fine-powder, use powder compressing machine that its pressure is thin slice, then thin slice is placed 200 ℃ of lower insulations 3 hours, obtain carbon/silicon nucleocapsid structure-PVDF matrix material, shown in Fig. 1 b.With the slice surfaces polishing, the surface-coated conductive silver glue can carry out the measurement of electrical properties after the oven dry.According to different ratio requirement, repeat aforesaid operations, make the matrix material of a series of different loading levels.Obtain the specific inductivity of matrix material with the rule of carbon/silicon nucleocapsid structure Material Filling quantitative change, shown in Fig. 2 a.The loading level of carbon/silicon nucleocapsid structure material conductor-insulator transition characteristic occurs near 19wt% the time, and this moment, specific inductivity reached 2030, and dielectric loss is 2.02.
Claims (3)
1. the polymer-based carbon high-dielectric composite material of carbon containing/silicon nucleocapsid structure filler, it is characterized in that: described matrix material is composited by carbon/silicon nucleocapsid structure material and polymkeric substance.
2. a kind of preparation method who contains the polymer-based carbon high-dielectric composite material of nucleocapsid structure filler is provided.The steps include:
Get a certain amount of carbon/silicon nucleocapsid structure material, join in 20 milliliters of alcohol solvents, ultra-sonic dispersion 3 hours, the superpolymer powder that mixes certain mass continued ultra-sonic dispersion 2 hours, with 80 ℃ of dryings of suspension liquid of obtaining, grind after, obtain trickle powder, use powder compressing machine that it is pressed and be thin slice.Then thin slice is placed 200 ℃ of lower insulations 3 hours, obtain the polymer matrix composite of carbon/silicon nucleocapsid structure Material Filling.
3. claim 1 and 2 described nucleocapsid structure materials comprise that all are take the nucleocapsid structure material of carbon material as nuclear.Polymer materials is all dielectric polymer materials that comprise PVDF.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104151751A (en) * | 2014-06-09 | 2014-11-19 | 中国石油大学(华东) | Carbon nano tube/amorphous carbon core-shell structure-polymer dielectric composite material |
| CN105367959A (en) * | 2015-10-27 | 2016-03-02 | 北京航空航天大学 | Core shell structure powder and method for preparing polymer-based dielectric composite material thereof |
| CN109971153A (en) * | 2019-04-04 | 2019-07-05 | 上海安费诺永亿通讯电子有限公司 | A kind of polymer matrix composites and preparation method thereof |
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| JPS58163726A (en) * | 1982-03-17 | 1983-09-28 | Unitika Ltd | Electroconductive conjugate fiber |
| CN101677033A (en) * | 2008-09-19 | 2010-03-24 | 深圳先进技术研究院 | Polymer-matrix composite dielectric material and plate capacitor |
| CN102174236A (en) * | 2011-03-16 | 2011-09-07 | 哈尔滨师范大学 | Preparation method of polyvinylidene fluoride-based composite with high dielectric constant |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58163726A (en) * | 1982-03-17 | 1983-09-28 | Unitika Ltd | Electroconductive conjugate fiber |
| CN101677033A (en) * | 2008-09-19 | 2010-03-24 | 深圳先进技术研究院 | Polymer-matrix composite dielectric material and plate capacitor |
| CN102174236A (en) * | 2011-03-16 | 2011-09-07 | 哈尔滨师范大学 | Preparation method of polyvinylidene fluoride-based composite with high dielectric constant |
Non-Patent Citations (1)
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| 李淑琴等: "多壁碳纳米管填充聚偏氟乙烯复合薄膜的介电性能", 《南京航空航天大学学报》, vol. 40, no. 01, 15 February 2008 (2008-02-15) * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104151751A (en) * | 2014-06-09 | 2014-11-19 | 中国石油大学(华东) | Carbon nano tube/amorphous carbon core-shell structure-polymer dielectric composite material |
| CN104151751B (en) * | 2014-06-09 | 2016-08-17 | 中国石油大学(华东) | A kind of CNT/amorphous carbon nucleocapsid structure-Polymeric dielectric composite |
| CN105367959A (en) * | 2015-10-27 | 2016-03-02 | 北京航空航天大学 | Core shell structure powder and method for preparing polymer-based dielectric composite material thereof |
| CN109971153A (en) * | 2019-04-04 | 2019-07-05 | 上海安费诺永亿通讯电子有限公司 | A kind of polymer matrix composites and preparation method thereof |
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Application publication date: 20130403 |