CN103450463A - Preparation method of poly(3,4-ethylenedioxythiophene)/reduced graphene oxide/Co3O4 (PEDOT-RGO-Co3O4) nano wave-absorbing material - Google Patents
Preparation method of poly(3,4-ethylenedioxythiophene)/reduced graphene oxide/Co3O4 (PEDOT-RGO-Co3O4) nano wave-absorbing material Download PDFInfo
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- CN103450463A CN103450463A CN2013103829089A CN201310382908A CN103450463A CN 103450463 A CN103450463 A CN 103450463A CN 2013103829089 A CN2013103829089 A CN 2013103829089A CN 201310382908 A CN201310382908 A CN 201310382908A CN 103450463 A CN103450463 A CN 103450463A
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Abstract
The invention provides a preparation method of a poly(3,4-ethylenedioxythiophene)/reduced graphene oxide/Co3O4 (PEDOT-RGO-Co3O4) nano wave-absorbing material. The PEDOT-RGO-Co3O4 composite material is prepared by adopting a three-step method; detection results show that quantity of oxygen-containing functional groups in graphene oxide (GO) of the PEDOT-RGO-Co3O4 nano composite material is greatly reduced, and GO is reduced into reduced graphene oxide (RGO); strong interaction exists between PEDOT and the RGO, and formed Co3O4 nano particles are distributed on the surface of PEDOT-RGO, and particle size of the Co3O4 nano particles is 5-15nm. According to the preparation method of the PEDOT-RGO-Co3O4 nano wave-absorbing material, the PEDOT-RGO-Co3O4 nano composite material is uniformly mixed with paraffin (in mass ratio of 1:1), mixture is pressed into an annular mould (with the height of 2.0mm, the outer diameter of 7.0mm and the inner diameter of 3.0mm) to prepare a sample, thickness is controlled to be 3.1mm, frequency is 7.1GHz, and the optimal wave-absorbing property is -46.4dB.
Description
Technical field
The present invention relates to the fabulous matrix material of a kind of absorbing property, relate to a kind of poly-3,4-ethylene dioxythiophene/Graphene/Co
3o
4the preparation method of nano wave-absorbing material.
Background technology
Poly-3,4 – ethylenedioxy thiophenes are a kind of novel thiophene derivants, and this polymkeric substance not only environmental stability is good, and has high conductivity, in all many-sides, obtains commercial application at home and abroad.
Graphene be a kind of have the bi-dimensional cellular nanostructure, by single carbon atom close-packed arrays, formed new carbon, it has larger specific surface area, good specific conductivity, mechanical stability and thermostability, therefore at aspects such as electronics, electrical condenser, mixture enhancings, all is widely used.
We have prepared poly-3,4 – ethylenedioxy thiophene/Graphenes/Co with three-step approach first
3o
4(PANI-RGO-Co
3o
4) nano composite material.Utilize FT-IR, XRD and TEM are characterized prepared nano composite material, and the nano composite material that we prepare is expected to possess application prospect widely at super capacitor material, electrode materials and absorbing material etc.
Chinese invention patent---application number is that CN102702929A relates to " a kind of chiral polyaniline antiradar coatings and preparation method ".The antiradar coatings absorbing property made by the method is not very outstanding, coating thickness 2mm left and right, and the 8-18GHz average reflectance is-10.124dB.
Summary of the invention
For avoiding prior art to obtain defect, the present invention proposes a kind of poly-3,4-ethylene dioxythiophene/Graphene claimed in claim 1/Co for preparing
3o
4the method of nano wave-absorbing material.
Technical scheme
A kind of poly-3,4 – ethylenedioxy thiophene/Graphenes claimed in claim 1/Co for preparing
3o
4the method of nano wave-absorbing material is characterized in that step is as follows:
Step 1: the ethylenedioxy thiophene of 0.2ml and 2ml concentrated sulfuric acid solution are added to ultrasonic 2h in the GO solution (1mg/ml) of 100ml, then add 0.95g (NH
4)
2s
2o
8, in ice bath, stir after 24h with deionized water wash for several times and be made into 100ml solution;
Step 2: by 1.4g CoCl
26H
2o adds above-mentioned solution, after stirring 2h, pours in the teflon-lined autoclave, then adds the H that 0.94g NaOH and 4ml massfraction are 30%
2o
2be placed in 160 ℃ of baking ovens and react 24h, after room temperature is cooling by the product of gained with deionized water wash for several times and be made into 100mL solution;
Step 3: the hydrazine hydrate solution that is 80% by the 0.1ml massfraction adds above-mentioned solution, use ethanol and deionized water wash for several times after reaction 24h in 95 ℃, then by products therefrom 60 ℃ of placement 24h in vacuum drying oven, obtain required poly-3,4 – ethylenedioxy thiophene/Graphenes/Co
3o
4nano composite material.
The consumption that above-mentioned each component consumption is every part.
In described step 1, the ethylenedioxy thiophene monomer purity is as far as possible high.
Beneficial effect
A kind of poly-3,4 – ethylenedioxy thiophene/Graphenes that the present invention proposes/Co
3o
4the preparation method of nano wave-absorbing material, prepared poly-3,4 – ethylenedioxy thiophene/Graphenes/Co with three-step approach
3o
4(PEDOT-RGO-Co
3o
4) nano composite material: detected result shows: PEDOT-RGO-Co
3o
4the oxygen-containing functional group quantity of graphite oxide in nano composite material (GO) significantly reduces, and GO has been reduced into Graphene (RGO); There is very strong interaction between PEDOT and RGO, and the Co formed
3o
4nanoparticle is distributed in the PEDOT-RGO surface, and its particle diameter is between 5-15nm.
The inventive method will be gathered 3,4 – ethylenedioxy thiophene/Graphenes/Co
3o
4nano composite material is evenly mixed (mass ratio 1:1) with paraffin, be pressed in ring mould (high 2.0mm, external diameter 7.0mm, internal diameter 3.0mm) and make sample, controls thickness 3.1mm, frequency 7.1GHz, preferably reach-46.4dB of absorbing property.
The accompanying drawing explanation
Fig. 1: poly-3,4 – ethylenedioxy thiophene/Graphenes/Co
3o
4the FT-IR spectrogram of nano wave-absorbing material;
Fig. 2: poly-3,4 – ethylenedioxy thiophene/Graphenes/Co
3o
4the XRD spectra of nano wave-absorbing material;
Fig. 3: poly-3,4 – ethylenedioxy thiophene/Graphenes/Co
3o
4the TEM figure of nano wave-absorbing material.
Fig. 4: poly-3,4 – ethylenedioxy thiophene/Graphenes/Co
3o
4the absorbing property of nano wave-absorbing material.
Embodiment
Now in conjunction with the embodiments, the invention will be further described for accompanying drawing:
1., 0.2ml ethylenedioxy thiophene monomer and 2ml concentrated sulfuric acid solution are added to ultrasonic 2h in the GO solution (1mg/ml) of 100ml embodiment 1:, then add 0.95g (NH
4)
2s
2o
8, in ice bath, stir after 24h with deionized water wash for several times and be made into 100ml solution; 2., by 1.4g CoCl
26H
2o adds above-mentioned solution, after stirring 2h, pours in the teflon-lined autoclave, then adds the H that 0.94g NaOH and 4ml massfraction are 30%
2o
2be placed in 160 ℃ of baking ovens and react 24h, after room temperature is cooling by the product of gained with deionized water wash for several times and be made into 100ml solution; 3., the hydrazine hydrate solution that is 80% by the 0.1ml massfraction adds above-mentioned solution, use ethanol and deionized water wash for several times after reaction 24h in 95 ℃, then by products therefrom 60 ℃ of placement 24h in vacuum drying oven, obtain required poly-3,4 – ethylenedioxy thiophene/Graphenes/Co
3o
4nano composite material.
1., 0.2ml ethylenedioxy thiophene monomer and 3ml concentrated sulfuric acid solution are added to ultrasonic 2h in the GO solution (1mg/ml) of 100ml embodiment 2:, then add 0.95g (NH
4)
2s
2o
8, in ice bath, stir after 24h with deionized water wash for several times and be made into 100ml solution; 2., by 1.4g CoCl
26H
2o adds above-mentioned solution, after stirring 2h, pours in the teflon-lined autoclave, then adds the H that 0.94g NaOH and 4ml massfraction are 30%
2o
2be placed in 160 ℃ of baking ovens and react 24h, after room temperature is cooling by the product of gained with deionized water wash for several times and be made into 100ml solution; 3., the hydrazine hydrate solution that is 80% by the 0.1ml massfraction adds above-mentioned solution, use ethanol and deionized water wash for several times after reaction 24h in 95 ℃, then by products therefrom 60 ℃ of placement 24h in vacuum drying oven, obtain required poly-3,4 – ethylenedioxy thiophene/Graphenes/Co
3o
4nano composite material.
Claims (1)
1. poly-3,4-ethylene dioxythiophene/Graphene/Co
3o
4the method of nano wave-absorbing material is characterized in that step is as follows:
Step 1: the 3,4-ethylene dioxythiophene monomer of 0.2ml and 2ml concentrated sulfuric acid solution are added to ultrasonic 2h in the GO solution of 100ml, then add 0.95g (NH
4)
2s
2o
8, in ice bath, stir after 24h with deionized water wash for several times and be made into 100ml solution; Described GO strength of solution is 1mg/ml;
Step 2: by 1.4g CoCl
26H
2o adds above-mentioned solution, after stirring 2h, pours in the teflon-lined autoclave, then adds the H that 0.94g NaOH and 4ml massfraction are 30%
2o
2be placed in 160 ℃ of baking ovens and react 24h, after room temperature is cooling by the product of gained with deionized water wash for several times and be made into 100ml solution;
Step 3: the hydrazine hydrate solution that is 80% by the 0.1ml massfraction adds above-mentioned solution, use ethanol and deionized water wash for several times after reaction 24h in 95 ℃, then by products therefrom 60 ℃ of placement 24h in vacuum drying oven, obtain required poly-3,4-ethylene dioxythiophene/Graphene/Co
3o
4nano composite material;
The consumption that above-mentioned each component consumption is every part.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104212131A (en) * | 2014-07-21 | 2014-12-17 | 中国人民解放军理工大学 | Graphene-polythiophene three-dimensional self-assembling-structured wave-absorbing material and preparation method thereof |
| CN104986808A (en) * | 2015-06-26 | 2015-10-21 | 江苏大学 | Preparation method and application of cobaltosic oxide/graphene aerogel composite material |
| CN105632787A (en) * | 2016-01-20 | 2016-06-01 | 安徽大学 | Preparation method of cobaltosic oxide/graphene nano composite electrode material for super capacitor |
| CN107057396A (en) * | 2017-01-24 | 2017-08-18 | 北京理工大学珠海学院 | A kind of preparation method of flexible absorbing material |
| WO2020119242A1 (en) * | 2018-12-13 | 2020-06-18 | 洛阳尖端技术研究院 | Ternary composite wave-absorbing agent and preparation method therefor |
| CN115197674A (en) * | 2022-08-31 | 2022-10-18 | 盐城工学院 | Cobaltosic oxide/nickel oxide/PEDOT wave-absorbing material and preparation method thereof |
| CN115340131A (en) * | 2022-08-31 | 2022-11-15 | 盐城工学院 | Preparation method of cobalt disulfide-polythiophene wave-absorbing material |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104212131A (en) * | 2014-07-21 | 2014-12-17 | 中国人民解放军理工大学 | Graphene-polythiophene three-dimensional self-assembling-structured wave-absorbing material and preparation method thereof |
| CN104986808A (en) * | 2015-06-26 | 2015-10-21 | 江苏大学 | Preparation method and application of cobaltosic oxide/graphene aerogel composite material |
| CN104986808B (en) * | 2015-06-26 | 2016-08-31 | 江苏大学 | A kind of preparation method and its usage of cobalt oxide/graphene aerogel composite |
| CN105632787A (en) * | 2016-01-20 | 2016-06-01 | 安徽大学 | Preparation method of cobaltosic oxide/graphene nano composite electrode material for super capacitor |
| CN107057396A (en) * | 2017-01-24 | 2017-08-18 | 北京理工大学珠海学院 | A kind of preparation method of flexible absorbing material |
| WO2020119242A1 (en) * | 2018-12-13 | 2020-06-18 | 洛阳尖端技术研究院 | Ternary composite wave-absorbing agent and preparation method therefor |
| CN111320968A (en) * | 2018-12-13 | 2020-06-23 | 洛阳尖端技术研究院 | Ternary composite wave absorbing agent and preparation method thereof |
| CN115197674A (en) * | 2022-08-31 | 2022-10-18 | 盐城工学院 | Cobaltosic oxide/nickel oxide/PEDOT wave-absorbing material and preparation method thereof |
| CN115340131A (en) * | 2022-08-31 | 2022-11-15 | 盐城工学院 | Preparation method of cobalt disulfide-polythiophene wave-absorbing material |
| CN115340131B (en) * | 2022-08-31 | 2023-06-02 | 盐城工学院 | Preparation method of cobalt disulfide-polythiophene wave-absorbing material |
| CN115197674B (en) * | 2022-08-31 | 2023-10-24 | 盐城工学院 | Tricobalt tetraoxide/nickel oxide/PEDOT wave-absorbing material and preparation method thereof |
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Application publication date: 20131218 |