CN102702745A - Preparation method of carbon nanotube/thermosetting resin composite material - Google Patents
Preparation method of carbon nanotube/thermosetting resin composite material Download PDFInfo
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- CN102702745A CN102702745A CN2012101982041A CN201210198204A CN102702745A CN 102702745 A CN102702745 A CN 102702745A CN 2012101982041 A CN2012101982041 A CN 2012101982041A CN 201210198204 A CN201210198204 A CN 201210198204A CN 102702745 A CN102702745 A CN 102702745A
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Abstract
The invention discloses a preparation method of a carbon nanotube/thermosetting resin composite material. The preparation method comprises the following steps of: uniformly mixing 100 parts by weight of thermosetting resin and 0.1-2 parts by weight of carbon nanotube to obtain prepolymer; dividing the prepolymer into a plurality of parts; taking one part of prepolymer, precuring at certain temperature and cooling to obtain a precured sheet; taking another part of prepolymer and pouring on the precured sheet, and then precuring; precuring the rest parts of prepolymer in steps in sequence to obtain a precured body; and curing and post-treating to obtain the carbon nanotube/thermosetting resin composite material. Compared with the carbon nanotube/thermosetting resin composite material prepared by one-time forming in the prior art, the composite material provided by the invention has the advantages of higher dielectric constant, lower dielectric loss angle tangent value, simple and practical preparation method, controllable process and suitability for large-scale production.
Description
Technical field
The present invention relates to a kind of preparation method of organic high molecular compound, particularly a kind of preparation method with carbon nanotube/thermoset ting resin composite of dielectric function.
Background technology
In all passive elements of electronic industry, multiple different functions such as electrical condenser is decoupled owing to having, bypass, filtering, energy transformation receive widely and paying close attention to.Have greater functionality and need embed electrical condenser in the printed electronic circuit inner cord with the electronic product of small volume more; In order to satisfy this requirement, the polymer matrix composite with high-k is able to use and gives birth to its good processibility with the circuit card favorable compatibility.
Conductor/polymer composites is the principal mode of preparation high dielectric constant material.Wherein, carbon nanotube has high specific surface area, excellent electroconductibility and thermal conductivity becomes one of the most promising conductor; And thermosetting resin becomes the matrix commonly used of Composite Preparation with its favorable manufacturability and excellent mechanical property.Therefore carbon nanotube/thermoset ting resin composite causes people's great interest aspect high dielectric constant material.But similar with other conductor/polymer composites, carbon nanotube/thermoset ting resin composite is ubiquity dielectric loss problem of higher also.High dielectric loss is not only wasted a large amount of energy, and shortens the work-ing life of equipment.
Before the present invention makes, bibliographical information a kind ofly utilize the technical scheme that natural sedimentation prepares the cyanate ester resin composite material of carbon nanotube (CNT) distribution gradient (referring to document: Hongyi Wu, Guozheng Liang; Aijuan Gu; Li Yuan. J. Mater. Chem. 2011,21,14838-14848); The composite material concurrent high-k and the low-dielectric loss that provide; Yet the difficult control of its preparation technology particularly faces bigger challenge in large-scale application.
Therefore, under the constant situation of the essentially consist of matrix material, how through setting up the novel method of Composite Preparation, the matrix material that obtains to have concurrently high-k and low-dielectric loss has important use value.
Summary of the invention
In order to overcome the problem that exists in the prior art, the object of the present invention is to provide a kind of simple, technology is controlled, is suitable for the method for scale operation carbon nanotube/thermoset ting resin composite.
The technical scheme that realization the object of the invention is taked provides a kind of preparation method of carbon nanotube/thermoset ting resin composite, comprises the steps:
(1) by weight, 100 parts of thermosetting resins and 0.1～2.0 part of carbon nanotube are mixed, under the pre-polymerization temperature condition of said thermosetting resin, obtain prepolymer; Prepolymer is divided into n part, n >=2, every part identical in quality or inequality;
(2) portion in n part prepolymer is carried out Procuring, obtain carbon nanotube/thermosetting resin Procuring sheet after the cooling;
(3) another part of getting in the prepolymer is cast on the Procuring sheet, carries out Procuring again; Repeat this step,, obtain a kind of Procuring body of carbon nanotube/thermoset ting resin composite all the other each parts proceed step by step Procuring successively in the prepolymer;
(4) by the curing and the aftertreatment technology condition of said thermosetting resin, the Procuring body that step (3) is obtained is cured and aftertreatment, promptly obtains a kind of carbon nanotube/thermoset ting resin composite.
Described carbon nanotube is a kind of without in surface treatment or surface treated SWCN, the multi-walled carbon nano-tubes, or its arbitrary combination.
Described thermosetting resin is self heat-setting resin; Like bimaleimide resin, cyanate ester resin and combination thereof.
The resin system that described thermosetting resin is formed for self can not be heated solidified resin and solidifying agent; The solidified resin that self can not be heated is an epoxy resin.
The mechanism of technical scheme of the present invention is: adopt carbon nanotube/thermoset ting resin composite multistep Procuring forming technique; The surface of the matrix material that obtains after per step Procuring moulding is a resin-rich layer; It has not only increased the generation probability of little electric capacity; And intercepted the direct contact of carbon nanotube, greatly reduce the probability that composite inner forms conductive path, thereby obtain having concurrently the matrix material of high-k and low-dielectric loss.
Compared with prior art, the beneficial effect obtained of the present invention is:
1, because the different microtexture of matrix material that has adopted multistep forming technique, the carbon nanotube/thermoset ting resin composite that makes to have to obtain with traditional one-step moulding has high-k and low-dielectric loss concurrently.
2, the preparation method of carbon nanotube/thermoset ting resin composite provided by the invention has characteristics simple, that technology is controlled and advantage, is suitable for scale operation.
Description of drawings
Fig. 1 is the carbon nanotube/cyanate ester resin composite material of embodiment of the invention preparation and the specific inductivity-frequency curve comparison diagram of layered carbon nano pipe/cyanate resin base composite material;
Fig. 2 is the carbon nanotube/cyanate ester resin composite material of embodiment of the invention preparation and the tangent of the dielectric loss angle value-frequency curve comparison diagram of layered carbon nano pipe/cyanate resin base composite material.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done and to further describe.
Embodiment 1
With the 0.02g multi-walled carbon nano-tubes, the 20g bisphenol A cyanate ester mixes, and stirs 1h in 85 ℃ of following sonic oscillations, obtains mixed solution, then with mixed solution at 150 ℃ of following pre-polymerization 2h.Pre-polymerization is divided into 2 equal portions with prepolymer after finishing.With wherein 1 part pour in the good mould of preheating, at 140 ℃ of following vacuum defoamation 30min.Then mould is put into baking oven,, obtain carbon nanotube/cyanate ester resin composite material Procuring sheet after the cooling at 180 ℃ of following Procuring 30min.
Remaining 1 part of prepolymer is cast on the Procuring sheet, behind 140 ℃ of following vacuum defoamation 30min, is cured and aftertreatment, obtain carbon nanotube/cyanate ester resin composite material according to 180 ℃ of technologies/2h+200 ℃/2h+220 ℃/2h and 240 ℃/4h.
Embodiment 2
With the 0.4g SWCN, the 20g bisphenol A cyanate ester mixes, and stirs 1h in 85 ℃ of following sonic oscillations, obtains mixed solution, then with mixed solution at 150 ℃ of following pre-polymerization 2h.Pre-polymerization is divided into 3 parts with prepolymer after finishing, and mass ratio is 2:1:1.With wherein 1 part pour in the good mould of preheating, at 140 ℃ of following vacuum defoamation 30min.Then mould is put into baking oven,, obtain carbon nanotube/cyanate ester resin composite material Procuring sheet A after the cooling at 180 ℃ of following Procuring 30min.
The 2nd part of prepolymer is cast on the above-mentioned Procuring sheet A,, obtains carbon nanotube/cyanate ester resin composite material Procuring sheet B after the cooling at 140 ℃ of following vacuum defoamation 30min.
The 3rd part of prepolymer is cast on the Procuring sheet B, behind 140 ℃ of following vacuum defoamation 30min, is cured and aftertreatment, obtain carbon nanotube/cyanate ester resin composite material according to 180 ℃ of technologies/2h+200 ℃/2h+220 ℃/2h and 240 ℃/4h.
Embodiment 3
With the 0.14g SWCN, the 20g bisphenol A cyanate ester mixes, and stirs 1h in 85 ℃ of following sonic oscillations, obtains mixed solution, then with mixed solution at 150 ℃ of following pre-polymerization 2h.Pre-polymerization is divided into 4 parts with prepolymer after finishing, and mass ratio is 2:1:2:1.With wherein 1 part pour in the good mould of preheating, at 140 ℃ of following vacuum defoamation 30min.Then mould is put into baking oven,, obtain carbon nanotube/cyanate ester resin composite material Procuring sheet A after the cooling at 180 ℃ of following Procuring 30min.
The 2nd part of prepolymer is cast on the above-mentioned Procuring sheet A,, obtains carbon nanotube/cyanate ester resin composite material Procuring sheet B after the cooling at 140 ℃ of following vacuum defoamation 30min.
The 3rd part of prepolymer is cast on the above-mentioned Procuring sheet B,, obtains carbon nanotube/cyanate ester resin composite material Procuring sheet C after the cooling at 140 ℃ of following vacuum defoamation 30min.
The 4th part of prepolymer is cast on the Procuring sheet C, behind 140 ℃ of following vacuum defoamation 30min, is cured and aftertreatment, obtain carbon nanotube/cyanate ester resin composite material according to 180 ℃ of technologies/2h+200 ℃/2h+220 ℃/2h and 240 ℃/4h.
Embodiment 4
With the 0.14g SWCN, 10g N, N '-4,4 '-diphenyl methane dimaleimide and 7.4g diallyl bisphenol monomer mix, with mixture at 150 ℃ of following pre-polymerization 2h.Pre-polymerization is divided into n part with prepolymer after finishing, and mass ratio is 1:2:3: ...: (n-1): n (n is a positive integer, in the present embodiment, and n=10).With wherein 1 part pour in the good mould of preheating, at 140 ℃ of following vacuum defoamation 30min.Then mould is put into baking oven,, obtain carbon nanotube/cyanate ester resin composite material Procuring sheet A1 after the cooling at 180 ℃ of following Procuring 30min.
The 2nd part of prepolymer is cast on the above-mentioned Procuring sheet A1,, obtains carbon nanotube/cyanate ester resin composite material Procuring sheet A2 after the cooling at 140 ℃ of following vacuum defoamation 30min.
The 3rd part of prepolymer is cast on the above-mentioned Procuring sheet A2,, obtains carbon nanotube/cyanate ester resin composite material Procuring sheet A3 after the cooling at 140 ℃ of following vacuum defoamation 30min.
Repeat above step, obtain Procuring sheet A (n-1).
N part prepolymer is cast on the Procuring sheet A (n-1), behind 140 ℃ of following vacuum defoamation 30min, is cured and aftertreatment, obtain carbon nanotube/cyanate ester resin composite material according to 180 ℃ of technologies/2h+200 ℃/2h+220 ℃/2h and 240 ℃/4h.
Embodiment 5
With the 0.1g multi-walled carbon nano-tubes, the 20g bisphenol A cyanate ester mixes, and stirs 1h in 85 ℃ of following sonic oscillations, obtains mixed solution, then with mixed solution at 150 ℃ of following pre-polymerization 2h.Pre-polymerization is divided into 2 equal portions with prepolymer after finishing.With wherein 1 part pour in the good mould of preheating, at 140 ℃ of following vacuum defoamation 30min.Then mould is put into baking oven,, obtain carbon nanotube/cyanate ester resin composite material Procuring sheet after the cooling at 180 ℃ of following Procuring 30min.
Remaining 1 part of prepolymer is cast on the Procuring sheet, behind 140 ℃ of following vacuum defoamation 30min, is cured and aftertreatment, obtain carbon nanotube/cyanate ester resin composite material according to 180 ℃ of technologies/2h+200 ℃/2h+220 ℃/2h and 240 ℃/4h.
Comparative example 1: with the 0.1g multi-walled carbon nano-tubes, the 20g bisphenol A cyanate ester mixes, and stirs 1h in 85 ℃ of following sonic oscillations, obtains mixed solution, then with mixed solution at 150 ℃ of following pre-polymerization 2h.Pre-polymerization is poured prepolymer in the good mould of preheating into, at 140 ℃ of following vacuum defoamation 30min after finishing.Again mould is put into baking oven, be cured and aftertreatment, obtain multi-walled carbon nano-tubes/cyanate ester resin composite material according to 180 ℃/2h+200 ℃/2h+220 ℃/2h and 240 ℃/4h.
Referring to accompanying drawing 1, it is the comparison diagram of specific inductivity-frequency curve of the carbon nanotube/cyanate ester resin composite material of present embodiment and comparative example 1 preparation.Can find out that by Fig. 1 both specific inductivity reduce along with the rising of frequency.But the matrix material that present embodiment makes demonstrates higher specific inductivity at low frequency range, and this mainly is to have formed a resin-rich layer in the matrix material because two steps were cast in, and forms more little electric capacity, helps the raising of specific inductivity.
Referring to accompanying drawing 2, it is the tangent of the dielectric loss angle value-frequency curve comparison diagram of the carbon nanotube/cyanate ester resin composite material of present embodiment and comparative example 1 preparation.Can find out by Fig. 2; Compare with the carbon nanotube/cyanate ester resin composite material of comparative example 1 preparation; The matrix material of present embodiment preparation demonstrates lower tangent of the dielectric loss angle value; For example, when 10Hz, the tangent of the dielectric loss angle value of the carbon nanotube/cyanate ester resin composite material of present embodiment and comparative example 1 preparation is respectively 12.1 and 187.3.
Embodiment 6
With the 0.2g SWCN, the 20g bisphenol A cyanate ester mixes, and stirs 1h in 85 ℃ of following sonic oscillations, obtains mixed solution, then with mixed solution at 150 ℃ of following pre-polymerization 2h.Pre-polymerization is divided into 3 parts with prepolymer after finishing, and mass ratio is 1:1:1.With wherein 1 part pour in the good mould of preheating, at 140 ℃ of following vacuum defoamation 30min.Then mould is put into baking oven,, obtain carbon nanotube/cyanate ester resin composite material Procuring sheet A after the cooling at 180 ℃ of following Procuring 30min.
The 2nd part of prepolymer is cast on the above-mentioned Procuring sheet A,, obtains carbon nanotube/cyanate ester resin composite material Procuring sheet B after the cooling at 140 ℃ of following vacuum defoamation 30min.
The 3rd part of prepolymer is cast on the Procuring sheet B, behind 140 ℃ of following vacuum defoamation 30min, is cured and aftertreatment, obtain carbon nanotube/cyanate ester resin composite material according to 180 ℃ of technologies/2h+200 ℃/2h+220 ℃/2h and 240 ℃/4h.
Embodiment 7
With 0.5g acidifying multi-walled carbon nano-tubes, 20g epoxy resin (E-51) stirs 1h at 60 ℃ of following sonic oscillations, obtains mixed solution, then will add 0.8g triethylene diamine (solidifying agent).Stir after 10 minutes, with prepolymer be divided into 2 parts, mass ratio is 1:2.With wherein 1 part pour in the good mould of preheating, at 60 ℃ of following vacuum defoamation 20min.In 80 ℃ of following Procuring 30min, obtain carbon nano tube/epoxy resin Procuring sheet after the cooling then.
Remaining a prepolymer is cast on the Procuring sheet, behind 60 ℃ of following vacuum defoamation 30min,, obtains the carbon nano tube/epoxy resin matrix material according to being cured and aftertreatment of 80 ℃ of technologies/2h+100 ℃/2h+120 ℃/2h+150 ℃/4h.
With the epoxidised SWCN of 0.05g, 16g Cyclopeutadiene type cyanate and 4g N, N '-4,4 '-diphenyl methane dimaleimide mixes, at 150 ℃ of following pre-polymerization 2h.After pre-polymerization finishes, with prepolymer be divided into 2 parts, mass ratio is 1:2.With wherein 1 part pour in the good mould of preheating, at 140 ℃ of following vacuum defoamation 30min.At last mould is put into baking oven,, obtain carbon nanotube/bismaleimides-cyanate resin Procuring sheet after the cooling at 180 ℃ of following Procuring 30min.
Remaining a prepolymer is cast on the Procuring sheet; Behind 140 ℃ of following vacuum defoamation 30min; Be cured and, obtain layered carbon nano pipe/bismaleimides-cyanate resin matrix material according to the technology of 180 ℃/2h+200 ℃/2h+220 ℃/2h at 240 ℃ of following aftertreatment 4h.
Embodiment 9
With the epoxidised SWCN of 0.5g, 0.5g acidifying multi-walled carbon nano-tubes, 16g Cyclopeutadiene type cyanate and 4g N, N '-4,4 '-diphenyl methane dimaleimide mixes, at 150 ℃ of following pre-polymerization 2h.Pre-polymerization is divided into 2 equal portions with prepolymer after finishing.With wherein 1 part pour in the good mould of preheating, at 140 ℃ of following vacuum defoamation 30min.Then mould is put into baking oven,, obtain carbon nanotube/cyanate ester resin composite material Procuring sheet after the cooling at 180 ℃ of following Procuring 30min.Remaining 1 part of prepolymer is cast on the Procuring sheet; Behind 140 ℃ of following vacuum defoamation 30min; Be cured and aftertreatment according to 180 ℃ of technologies/2h+200 ℃/2h+220 ℃/2h and 240 ℃/4h, obtain carbon nanotube/bismaleimides-cyanate resin matrix material.
Claims (6)
1. the preparation method of a carbon nanotube/thermoset ting resin composite is characterized in that comprising the steps:
(1) by weight, 100 parts of thermosetting resins and 0.1～2.0 part of carbon nanotube are mixed, under the pre-polymerization temperature condition of said thermosetting resin, obtain prepolymer; Prepolymer is divided into n part, n >=2, every part identical in quality or inequality;
(2) portion in n part prepolymer is carried out Procuring, obtain carbon nanotube/thermosetting resin Procuring sheet after the cooling;
(3) another part of getting in the prepolymer is cast on the Procuring sheet, carries out Procuring again; Repeat this step,, obtain a kind of Procuring body of carbon nanotube/thermoset ting resin composite all the other each parts proceed step by step Procuring successively in the prepolymer;
(4) by the curing and the aftertreatment technology condition of said thermosetting resin, the Procuring body that step (3) is obtained is cured and aftertreatment, promptly obtains a kind of carbon nanotube/thermoset ting resin composite.
2. the preparation method of a kind of carbon nanotube/thermoset ting resin composite according to claim 1; It is characterized in that: a kind of for without in surface treatment or surface treated SWCN, the multi-walled carbon nano-tubes of described carbon nanotube, or its arbitrary combination.
3. the preparation method of a kind of carbon nanotube/thermoset ting resin composite according to claim 1 is characterized in that: described thermosetting resin is self heat-setting resin.
4. the preparation method of a kind of carbon nanotube/thermoset ting resin composite according to claim 3 is characterized in that: described self heat-setting resin is bimaleimide resin, cyanate ester resin and combination thereof.
5. the preparation method of a kind of carbon nanotube/thermoset ting resin composite according to claim 1 is characterized in that: the resin system that described thermosetting resin is formed for self can not be heated solidified resin and solidifying agent.
6. the preparation method of a kind of carbon nanotube/thermoset ting resin composite according to claim 5, it is characterized in that: the described solidified resin that self can not be heated is an epoxy resin.
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Cited By (9)
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| CN103073847A (en) * | 2013-01-23 | 2013-05-01 | 苏州大学 | Modified carbon nano tube/thermosetting resin composite material and preparation method thereof |
| CN103194858A (en) * | 2013-04-23 | 2013-07-10 | 北京化工大学 | Elastomer composite with high dielectric constant and low dielectric loss and preparation method thereof |
| CN104893287A (en) * | 2015-06-01 | 2015-09-09 | 苏州大学 | Carbon nanotube/phenolphthalein-based polyether sulphone/cyanate resin composite material and preparation method |
| CN105482339A (en) * | 2016-01-16 | 2016-04-13 | 苏州大学 | Lithium salt/polyacrylonitrile/thermosetting resin composite and preparation method thereof |
| CN107141793A (en) * | 2017-06-15 | 2017-09-08 | 铜陵安博电路板有限公司 | A kind of low-dielectric loss type polymer matrix composites of ZnOw filling and preparation method thereof |
| CN109161195A (en) * | 2018-08-02 | 2019-01-08 | 北京空间飞行器总体设计部 | A kind of conductivity type carbon nanotube/cyanate composite material and preparation method thereof |
| CN109776832A (en) * | 2019-01-15 | 2019-05-21 | 苏州大学 | Three-decker polymer matrix composites and its application |
| CN110014541A (en) * | 2017-09-11 | 2019-07-16 | 苏州大学 | Four-layer structure polymer matrix composites |
| CN110076946A (en) * | 2017-09-11 | 2019-08-02 | 苏州大学 | Three-decker polymer matrix composites presoma and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103073847A (en) * | 2013-01-23 | 2013-05-01 | 苏州大学 | Modified carbon nano tube/thermosetting resin composite material and preparation method thereof |
| CN103194858A (en) * | 2013-04-23 | 2013-07-10 | 北京化工大学 | Elastomer composite with high dielectric constant and low dielectric loss and preparation method thereof |
| CN103194858B (en) * | 2013-04-23 | 2015-08-05 | 北京化工大学 | Elastic composite of a kind of high dielectric constant and low dielectric loss and preparation method thereof |
| CN104893287A (en) * | 2015-06-01 | 2015-09-09 | 苏州大学 | Carbon nanotube/phenolphthalein-based polyether sulphone/cyanate resin composite material and preparation method |
| CN105482339A (en) * | 2016-01-16 | 2016-04-13 | 苏州大学 | Lithium salt/polyacrylonitrile/thermosetting resin composite and preparation method thereof |
| CN107141793A (en) * | 2017-06-15 | 2017-09-08 | 铜陵安博电路板有限公司 | A kind of low-dielectric loss type polymer matrix composites of ZnOw filling and preparation method thereof |
| CN110076946A (en) * | 2017-09-11 | 2019-08-02 | 苏州大学 | Three-decker polymer matrix composites presoma and preparation method thereof |
| CN110014541A (en) * | 2017-09-11 | 2019-07-16 | 苏州大学 | Four-layer structure polymer matrix composites |
| CN110076946B (en) * | 2017-09-11 | 2021-08-27 | 苏州大学 | Precursor for three-layer structure resin-based composite material and preparation method thereof |
| CN110014541B (en) * | 2017-09-11 | 2021-08-27 | 苏州大学 | Resin-based composite material with four-layer structure |
| CN109161195A (en) * | 2018-08-02 | 2019-01-08 | 北京空间飞行器总体设计部 | A kind of conductivity type carbon nanotube/cyanate composite material and preparation method thereof |
| CN109776832A (en) * | 2019-01-15 | 2019-05-21 | 苏州大学 | Three-decker polymer matrix composites and its application |
| CN109776832B (en) * | 2019-01-15 | 2021-03-02 | 苏州大学 | Three-layer structure resin-based composite material and application thereof |
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