CN103012791A - Preparation method of polypyrrole/graphene sheet/nickel oxide nano composite conductive material - Google Patents
Preparation method of polypyrrole/graphene sheet/nickel oxide nano composite conductive material Download PDFInfo
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- CN103012791A CN103012791A CN2012105776471A CN201210577647A CN103012791A CN 103012791 A CN103012791 A CN 103012791A CN 2012105776471 A CN2012105776471 A CN 2012105776471A CN 201210577647 A CN201210577647 A CN 201210577647A CN 103012791 A CN103012791 A CN 103012791A
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Abstract
The invention provides a polypyrrole/graphene sheet/nickel oxide nano composite conductive material and a preparation method thereof, belonging to the technical field of composite materials. By using alcohol as a medium, polyethylene glycol-400 as a dispersing agent, p-toluenesulfonic acid as a doping agent, and FeCl3 as an initiating agent, a graphene sheet, nano nickel oxide and polypyrrole monomers are polymerized under the ultrasonic condition to ensure that the polypyrrole and the nickel oxide nano particles are uniformly dispersed on the surface of a GNS (Graphene Nano Sheet) and the GNS is completely wrapped, thus the problem of agglomeration during polypyrrole agglomeration is solved, and the conduction property of the polypyrrole is effectively improved.
Description
Technical field
The invention belongs to technical field of composite materials, relate to the preparation of the nano combined electro-conductive material of a kind of polypyrrole base, relate in particular to a kind of take polypyrrole (PPy) as main body, the preparation method take graphene nano thin slice (GNS), nickel oxide (NiO) as the three-phase composite electro-conductive material of filler.
Background technology
The Conductive Polymer Material Polypyrrole (PPy) that contains conjugated double bond is compared with other conducting polymer composites higher conductive capability and thermostability, easily the characteristics such as synthetic are widely used in making biological inductor, functional molecular film, secondary cell and nonlinear optical device etc.Generally, the polypyrrole quality crisp, molten not insoluble, can not process.For the processing characteristics of improving polypyrrole, the conductivity that improves polypyrrole, by disperseing different functional properties conductivity fillers in the polypyrrole matrix, to form polypyrrole/inorganic layer composite conducting material, and the type that the performance of composite conducting material can be by the conductive filler material material, amount of filler, filler surface-functionalized etc. and can well being controlled.
The graphene nano thin slice is regarded as a kind of have advantage and application prospect conductive filler material owing to the laminated structure that has kept natural graphite has higher specific surface area, lower diafiltration threshold values and higher electroconductibility.Therefore the graphene nano thin slice is distributed to the polypyrrole/graphene thin slice nano composite material that obtains in the polypyrrole has good conductivity and workability.But in order further to improve polypyrrole/graphene thin slice nano composite material chemical property, introduce at present the focus that metal simple-substance or metal oxide become a research on the basis of two-phase composite material.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of polypyrrole/graphene thin slice/nickel oxide nano composite conducting material.
The preparation method of polypyrrole/graphene thin slice of the present invention/nickel oxide nano composite conducting material is take ethanol as medium, take PEG-4000 as dispersion agent, and take tosic acid as doping agent, FeCl
3Be initiator, graphene platelet, nano-nickel oxide, pyrrole monomer 0 ~ 5 ℃ of lower ultrasonic polymerization, are obtained polypyrrole/graphene thin slice/nickel oxide nano conducing composite material.Its concrete preparation technology is as follows:
With graphene platelet, nano-nickel oxide, pyrrole monomer and PEG-4000 ultra-sonic dispersion in dehydrated alcohol; Under 0 ~ 5 ℃, in system, add tosic acid, ultra-sonic dispersion 5 ~ 10min; Add again FeCl
3React 2 ~ 4h under the solution, ultrasound condition; Leave standstill, suction filtration, washing, drying gets polypyrrole/graphene thin slice/nickel oxide nano conducing composite material.
Wherein, the mass ratio of graphene platelet, pyrrole monomer, nano-nickel oxide is 1:8:3 ~ 1:18:18.
The consumption of described PEG-4000 is 1 ~ 2 times of pyrrole monomer quality.
5 ~ 20% of the add-on pyrrole monomer quality of described tosic acid.
Described FeCl
3The concentration of solution is 0.3 ~ 0.7mol/L, and FeCl
3Amount be 9 ~ 18 times of pyrrole monomer quality.
Below by scanning electron microscope, FTIR structure and the property of the PPy/GNS/NiO composite conducting material of the present invention's preparation are carried out analytic explanation.
1, electronic microscope photos
Fig. 1 is the SEM photo of pure PPy.As seen from Figure 1, PPy is the spherical particle of sub-circular, and the size of spherical particle is more even, coheres disorderly mutually between particle, piles up and be built into netted " bridge " structure with space.
Fig. 2 is the SEM photo of matrix material PPy/GNS.Can be clear that from Fig. 2 a large amount of spherical PPy is dispersed in the surface of GNS, even particle size presents a kind of spherical PPy in the epontic trend of GNS.
Can find that by comparison diagram 1,2 more all even particle diameter is less than the particle of pure PPy for the spherical PPy particle in matrix material.Infer that the reason that the spherical PPy particle in the matrix material diminishes is to have larger lamella in the matrix material, the GNS of highly fragrant basal plane, so that be adsorbed in the surface of GNS, the effect of having served as substrate or " nuclear " at a large amount of pyrrole monomer of polymerization initial stage and oligopolymer by electrostatic interaction.Therefore, pyrroles's polyreaction is controlled in certain scope, greatly reduces the collision polymerization probability between oligopolymer, the monomer, and then reduced the effect of speed of reaction, refinement polymer beads.
Fig. 3 is the SEM photo of PPy/GNS/NiO.As can see from Figure 3, polypyrrole and NiO nano particle are dispersed in the surface of GNS uniformly, and in GNS is coated on fully.The existence of a small amount of GNS makes nano-nickel oxide obtain good dispersion, the reunion of the nano particle that greatly reduces.
In sum, in the PPy/GNS/NiO conducing composite material of the present invention's preparation, nano NiO is dispersed in the middle of the GNS; Polypyrrole is grown in surface and the edge of GNS, and in GNS is coated on fully.
2, FTIR spectrum analysis
Fig. 4 is the FTIR spectrogram of PPy, NiO and PPy/GNS/NiO matrix material.Wherein (a) is the collection of illustrative plates of NiO, at 3429 cm
1Absorption peak and 1629 cm at place
1The weak absorption at place can be summed up as stretching vibration and the flexural vibration of planar water, at 467 cm
1Near the stretching vibration absorption peak of Ni-O appears.(b) be the spectrogram of pure polypyrrole, 3432 cm
-1For the N-H stretching vibration absorption peak on the pyrrole ring, at 1523 cm
-1The place is the flexible peak of C=C and C-C, is positioned at 1428 cm
-1Place's characteristic peak is the C-N stretching vibration peak of conjugation.At 1385 cm
-1The broad peak at place is the C-H vibration peak.1041 cm
-1The place is the vibration peak of S=O, proves that tosic acid has been doped among the PPy.(c) be the PPy/GNS/NiO spectrogram, they and PPy peak shape are closely similar, are some red shift of position with respect to the peak.This mainly is because small-size effect and the quantum size effect of GNS and NiO cause.In the recombination process of PPy and Graphene, there is the combination of chemical bond between them, can affect the vibrational frequency of the atom of with it combination, and polypyrrole has a kind of molecular structure of pi-conjugated chain, thisly affect the existence that meeting builds along with large π and affect the vibrational frequency of whole molecular chain, cause red shift.These phenomenons show that obviously PPy is not the simple physical coating to GNS, also exist simultaneously the combination of chemical bond, and this is just so that this complex method is more reliable, and performance also will be more stable.
3, the analysis of conductivity
The specific conductivity of PPy/GNS/NiO matrix material when table 1 is pure PPy, NiO, PPy/NiO, PPy/GNS and different NiO content.Can find out from the data of table 1, along with NiO content is brought up to 24.39 S/cm from 0 specific conductivity that is increased to 48.7%, PPy/GNS/NiO matrix material from 2 S/cm.When NiO content is low, be not clearly to the raising of electric conductivity, but when the content of NiO further increases, the specific conductivity of matrix material will increase considerably.This is owing to when the content of NiO is little, exist each other larger spacing in matrix material, can not form good conductive network, and very limited to the contribution of specific conductivity, conductive path is mainly provided by PPy and GNS.Continuous increase along with NiO content, NiO just can the form with conductive network in matrix material gradually exist, a large amount of conductive channels is provided, when the content of NiO is increased to 48.7%, just can reach to ooze and ooze territory filter value in the territory filter theory, so that significantly improving appears in the electroconductibility of matrix material.Therefore, in the conducing composite material of the present invention, in the content of NiO was controlled at 10 ~ 65.6% scope, the electric conductivity of conducing composite material was 2.00 S/cm in the electric conductivity of the pure PPy of 11.89 ~ 24.39 S/cm().
Table 1 is the specific conductivity of the PPy/GNS/NiO matrix material of different Ni O content
| Sample | PPy (%) | NiO(%) | GNS (%) | Specific conductivity (S/cm) |
| 1 | 100 | 0 | 0 | 2.00 |
| 2 | 0 | 100 | 0 | _ |
| 3 | 97 | 0 | 3 | 11.00 |
| 4 | 90 | 10 | 0 | 9.62 |
| 5 | 87.3 | 10 | 2.7 | 11.89 |
| 6 | 80.5 | 19.5 | 2.7 | 14.49 |
| 7 | 48.6 | 48.7 | 2.7 | 24.39 |
| 8 | 39.7 | 65.6 | 2.7 | 15.38 |
In sum, the present invention is take polypyrrole as matrix, take GNS and NiO as filler, under ultrasound condition, make polypyrrole and NiO nanoparticle be evenly distributed on the surface of GNS, and in GNS was coated on fully, the agglomeration traits when not only having solved pyrroles's polymerization had also improved the conductivity of polypyrrole effectively.
Description of drawings
Fig. 1 is the SEM photo of pure PPy;
Fig. 2 is the SEM photo of PPy/GNS matrix material;
Fig. 3 is the SEM photo of PPy/GNS/NiO matrix material;
Fig. 4 is the FTIR spectrogram of PPy/GNS/NiO matrix material.
Embodiment
Be elaborated below by preparation and the conductivity of specific embodiment to polypyrrole/graphene thin slice of the present invention/nickel oxide nano conducing composite material.
Embodiment 1
1. the preparation of graphene platelet (GNS): take by weighing 1g 200 purpose expansible black leads, place retort furnace, in 950 ~ 1050 ℃ of lower expanded 10 ~ 15s of temperature, make expanded graphite.Take orthodichlorobenzene as solvent, with the ultrasonic 3 ~ 4h that peels off of expanded graphite, filtration, washing, drying get GNS again.
2. the preparation of nano NiO: in there-necked flask, add 50mL 0.2mol/L NiSO
46H
2O is warming up to 70 ~ 80 ℃ under ultrasound condition; Regulate pH value to 10 ~ about 12 with 0.4mol/L KOH solution, continue ultrasonic reaction 3 ~ 5h; Cooling 6 ~ 12h, centrifugation, the distilled water repetitive scrubbing is extremely without SO
4 2-(use BaCl
2Check), uses at last absolute ethanol washing, behind the dry 24h, grind, then at 350 ℃ of calcining 1 ~ 2h, obtain the NiO that particle diameter is 1 ~ 3nm.
3. the preparation of PPy/GNS/NiO: get 0.015g GNS, 0.05 g NiO, 0.5g pyrrole monomer and 1 ml PEG-4000 add 6 ~ 10mL dehydrated alcohol in reactor, ultrasonic it are uniformly dispersed; Under condition of ice bath, add the 0.4g tosic acid, ultra-sonic dispersion 5min adds 50mL 0.34mol/L FeCl
3Solution, ultrasonic reaction 2 ~ 4 hours, hold over night, suction filtration, to wash to filtrate be colourless, drying gets the PPy/GNS/NiO conducing composite material.
The electric conductivity of PPy/GNS/NiO conducing composite material is 11.89 S/cm.
Embodiment 2
Nanometer GNS is identical with embodiment 1 with the preparation of nano NiO.
3. the preparation of PPy/GNS/NiO: get 0.016g GNS, 0.1 g NiO, 0.5g pyrrole monomer and 1 ml PEG-4000 add 6 ~ 10mL dehydrated alcohol in reactor, ultrasonic it are uniformly dispersed; Under condition of ice bath, add the 0.4g tosic acid, continue ultra-sonic dispersion 5min; Add 50mL 0.34mol/L FeCl
3Solution, ultrasonic reaction 2 ~ 4 hours, hold over night, suction filtration, to wash to filtrate be colourless, drying gets the PPy/GNS/NiO conducing composite material.
The electric conductivity of PPy/GNS/NiO conducing composite material is 14.49 S/cm.
Embodiment 3
Nanometer GNS is identical with embodiment 1 with the preparation of nano NiO.
The preparation of PPy/GNS/NiO: get 0.028g GNS, 0.5g NiO, 0.5g pyrrole monomer and 1ml PEG-4000 add 6 ~ 10mL dehydrated alcohol in reactor, ultrasonic it are uniformly dispersed; Under condition of ice bath, add the 0.4g tosic acid, ultra-sonic dispersion 8min; Add 50mL 0.34mol/L FeCl
3Solution, ultrasonic reaction 2 ~ 4 hours, hold over night, suction filtration, to wash to filtrate be colourless, drying gets the PPy/GNS/NiO conducing composite material.
The electric conductivity of PPy/GNS/NiO conducing composite material is 24.39 S/cm.
Embodiment 4
Nanometer GNS is identical with embodiment 1 with the preparation of nano NiO.
The preparation of PPy/GNS/NiO: get 0.013g GNS, 0.5g NiO, 0.25g pyrrole monomer and 0.5ml PEG-4000 add 6 ~ 10mL dehydrated alcohol in reactor, ultrasonic it are uniformly dispersed; Under condition of ice bath, add the 0.2g tosic acid, ultra-sonic dispersion 10min; Add 25mL 0.34mol/L FeCl
3Solution, ultrasonic reaction 2 ~ 4 hours, hold over night, suction filtration, to wash to filtrate be colourless, drying gets the PPy/GNS/NiO conducing composite material.
The electric conductivity of PPy/GNS/NiO conducing composite material is 15.38 S/cm.
Claims (6)
1. the preparation method of polypyrrole/graphene thin slice/nickel oxide nano composite conducting material, as medium take ethanol, take PEG-4000 as dispersion agent, take tosic acid as doping agent, iron trichloride is initiator, graphene platelet, nano-nickel oxide, pyrrole monomer 0 ~ 5 ℃ of lower ultrasonic polymerization, are obtained polypyrrole/graphene thin slice/nickel oxide nano conducing composite material.
2. the preparation method of polypyrrole/graphene thin slice/nickel oxide nano composite conducting material as claimed in claim 1 is characterized in that: with graphene platelet, nano-nickel oxide, pyrrole monomer and PEG-4000 ultra-sonic dispersion in dehydrated alcohol; Under 0 ~ 5 ℃, in system, add tosic acid, ultra-sonic dispersion 5 ~ 10min; Add again liquor ferri trichloridi, react 2 ~ 4h under the ultrasound condition; Leave standstill, suction filtration, washing, drying gets polypyrrole/graphene thin slice/nickel oxide nano conducing composite material.
3. the preparation method of polypyrrole/graphene thin slice/nickel oxide nano composite conducting material as claimed in claim 1 or 2, it is characterized in that: described graphene platelet, pyrrole monomer, nano-nickel oxide mass ratio are 1:8:3 ~ 1:18:18.
4. the preparation method of polypyrrole/graphene thin slice/nickel oxide nano composite conducting material as claimed in claim 1 or 2, it is characterized in that: the consumption of described PEG-4000 is 1 ~ 2 times of pyrrole monomer quality.
5. the preparation method of polypyrrole/graphene thin slice/nickel oxide nano composite conducting material as claimed in claim 1 or 2 is characterized in that: 5 ~ 20% of the add-on pyrrole monomer quality of described tosic acid.
6. the preparation method of polypyrrole/graphene thin slice/nickel oxide nano composite conducting material as claimed in claim 1 or 2, it is characterized in that: the amount of described iron trichloride is 9 ~ 18 times of pyrrole monomer quality.
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Cited By (6)
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| CN103871757A (en) * | 2014-03-21 | 2014-06-18 | 扬州大学 | Method for preparing high-capacitance polyaniline and nickel oxide composite electrode material |
| CN103887075A (en) * | 2014-04-11 | 2014-06-25 | 电子科技大学 | Method for manufacturing high-specific-capacity electrode thin film |
| CN106784710A (en) * | 2016-12-28 | 2017-05-31 | 广东工业大学 | A kind of carbon@metal oxide@metals/three-dimensional porous graphene composite material of core shell structure and its preparation method and application |
| CN107099055A (en) * | 2017-04-26 | 2017-08-29 | 常州大学 | A kind of preparation method of tungstic acid/polypyrrole/graphene composite material by template of attapulgite |
| CN107706000A (en) * | 2017-11-15 | 2018-02-16 | 齐鲁工业大学 | A kind of flower ball-shaped nickel oxide/polypyrrole/graphene composite material and preparation method thereof |
| CN108409963A (en) * | 2018-04-19 | 2018-08-17 | 太仓美克斯机械设备有限公司 | A kind of preparation method of anti-oxidant Polypyrrole Conducting Materials |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103871757A (en) * | 2014-03-21 | 2014-06-18 | 扬州大学 | Method for preparing high-capacitance polyaniline and nickel oxide composite electrode material |
| CN103871757B (en) * | 2014-03-21 | 2016-08-17 | 扬州大学 | High-capacitance polyaniline and the preparation method of nickel oxide combination electrode material |
| CN103887075A (en) * | 2014-04-11 | 2014-06-25 | 电子科技大学 | Method for manufacturing high-specific-capacity electrode thin film |
| CN106784710A (en) * | 2016-12-28 | 2017-05-31 | 广东工业大学 | A kind of carbon@metal oxide@metals/three-dimensional porous graphene composite material of core shell structure and its preparation method and application |
| CN106784710B (en) * | 2016-12-28 | 2019-07-09 | 广东工业大学 | A kind of carbon@metal oxide@metal/three-dimensional porous graphene composite material of core-shell structure and its preparation method and application |
| CN107099055A (en) * | 2017-04-26 | 2017-08-29 | 常州大学 | A kind of preparation method of tungstic acid/polypyrrole/graphene composite material by template of attapulgite |
| CN107099055B (en) * | 2017-04-26 | 2018-08-28 | 常州大学 | It is a kind of using attapulgite as the preparation method of tungstic acid/polypyrrole/graphene composite material of template |
| CN107706000A (en) * | 2017-11-15 | 2018-02-16 | 齐鲁工业大学 | A kind of flower ball-shaped nickel oxide/polypyrrole/graphene composite material and preparation method thereof |
| CN107706000B (en) * | 2017-11-15 | 2019-08-09 | 齐鲁工业大学 | Flower ball-shaped nickel oxide/polypyrrole/graphene composite material and preparation method thereof |
| CN108409963A (en) * | 2018-04-19 | 2018-08-17 | 太仓美克斯机械设备有限公司 | A kind of preparation method of anti-oxidant Polypyrrole Conducting Materials |
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Application publication date: 20130403 |