CN102544501A - Method for preparing polypyrrole nanometer wire-graphene composite material - Google Patents
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
Provided is a method for preparing a polypyrrole nanometer wire-graphene composite material. Pyrrole monomer and graphene powder are added in prepared disodium hydrogen phosphate lithium perchlorate aqueous solution with certain concentration according to certain proportion, even suspension liquid is obtained after ultrasonic dispersion, an experiment is carried out in a three-electrode system controlled by an electrochemical workstation, an electrochemical method is adopted, and the polypyrrole nanometer wire-graphene composite material is obtained through polymerization on an electric conduction substrate. The method is simple in process, short in time, controllable in operation procedure and low in cost. The composite material is high in conductivity rate, capable of serving as electrode materials to be applied to a fuel battery, capable of being applied to supercapacitors, lithium batteries, sensors and the like.
Description
Technical field
The present invention relates to a kind of preparation method of polypyrrole nano line-graphene composite material, particularly make electrolyte, form the method for polypyrrole nano line/graphene composite material through electrochemical method with sodium hydrogen phosphate and lithium perchlorate.
Background technology
Have the conducting high polymers thing polypyrrole of conjugated pi-key because have higher conductivity, than electric capacity, good electrochemical stability, environmental stability and biocompatibility; Be widely used in fields such as electrode material, ultracapacitor, biology sensor, since finding, received researcher's attention always.Polypyrrole nano line is except that the characteristic that possesses common membranaceous polypyrrole, and conductivity exceeds an one magnitude than common polypyrrole usually and (sees document " Controlling the Morphology of Electronically Conductive Polymers ", Penner; R. M., Martin, C. R; J. Electrochem. Soc., 133,1986; 2206-2207), make polypyrrole nano line be applied in the advantage that has more on the electrode.In order to obtain the new material of high conductivity, electrochemical stability and superior mechanical performance, the compound of research polypyrrole nano line and other nano materials has become a big research focus.Graphene is by the compact arranged two-dimension single layer structure of carbon atom hexagonal structure; It is the elementary cell that constitutes other graphite materials; It can warpage becomes the fullerene of zero dimension, has been rolled into the CNT of one dimension or has piled three-dimensional graphite, since utilizing the mechanical stripping method to obtain the Graphene of individual layer; Because it has extremely excellent electricity, mechanics and mechanical performance, become the focus of material science research rapidly.
At present, among the preparation method about polypyrrole/graphene composite material, adopt chemical method mostly, as at 1. " Electrochemical performance of a graphene-polypyrrole nanocomposite as a supercapacitor electrode " (Saswata Bose of document; Nam Hoon Kim, Tapas Kuila, Kin-tak Lau; Joong Hee Lee, Nanotechnology, 22; 2011,295202) and 2. " Enhanced capacitance and rate capability of graphene/polypyrrole composite as electrode material for supercapacitors " (Dacheng Zhang, Xiong Zhang; Yao Chen, Peng Yu, Changhui Wang; Yanwei Ma, Journal of Power Sources, 196; 2011,5990-5996) in, the polypyrrole/graphene compound is formed by Graphene and pyrrole monomer in-situ polymerization.Be that a certain amount of pyrrole monomer is dissolved in the ethanol water and with after ultrasonic scattered Graphene mixes, adds FeCl
3Form.Document 1. and 2. in preparation method's main difference be that Graphene was handled by kayexalate (Na-PSS) during document 1., and document 2. in Graphene do not handled by Na-PSS.At 3. " Preparation of graphene/polypyrrole composites for electrochemical capacitors " (Yongqing Han of document; Bing Ding, Xiaogang Zhang, Journal of New Materials for Electrochemical Systems 13; 315-320; 2010) in, the preceding step of the preparation process of polypyrrole/graphene compound is 1. more similar with 2. with document, is promptly formed by Graphene and pyrrole monomer in-situ polymerization; But after a certain amount of pyrrole monomer joins ultrasonic scattered Graphene mixing, form and add oxidant ammonium persulfate (APS).At 4. " graphene complex is containing the application study in the Hg waste water treatment " (Zhang Jinghuang of document; West, Fujian Vocationl Technical College journal; The 115th page of the 13rd the 2nd phase of volume) in; Adopt the synthetic polypyrrole of ammonium hydrogen sulfate chemical polymerization method, be about to graphene oxide and polypyrrole and be distributed to according to a certain percentage in the water, add hydrogen sulfate amine and hydrazine hydrate respectively and form.At 5. " In-situ synthesis and characterization of electrically conductive polypyrrole/graphene nanocomposites " (Saswata Bose, Tapas Kuila, Md. Elias Uddin of document; Nam Hoon Kim, Alan K.T. Lau, Joong Hee Lee; Polymer, 51,2010; 5921-5928), adopting behind graphene oxide and the pyrrole monomer in-situ polymerization also, electronation forms.Be after a certain amount of pyrrole monomer is dissolved in the ethanol water and mixes with ultrasonic scattered graphene oxide, to add FeCl
3Solution synthesizes after polypyrrole/graphene oxide compound, adds to form after hydrazine reduces again.The polypyrrole/graphene compound also can be made by in-situ chemical oxidation polymerization method (sees 6. " Synthesis of novel hierarchical graphen/polypyrrole nanosheet composites and their superior electrochemical performance " (Chaohe Xu of document; Jing Sun; Lian Gao; J. Mater. Chem, 2011,21 11253); Be ammoniacal liquor join be uniformly dispersed in the suspension of glucose and graphene oxide the back and separate after, add pyrrole monomer again; Hydrochloric acid and APS are taken up in order of priority to join in the reactant liquor successively and get final product afterwards, and the polypyrrole that is obtained exists with the form of nanometer sheet.The said method of before is different; The composite material of polypyrrole/graphene can also join behind the graphene nano fiber of ultrasonic dispersion electrochemistry constant voltage electropolymerization through pyrrole monomer and form and (see document 7. " Stacked graphene nanofibers doped polypyrrole nanocomposites for electrochemical sensing "; Claire L. Scott; Guanjia Zhao, Martin Pumera, Electrochemistry Communications 12; 2010,1788-1791).
Have about the patent of the preparation this respect of polypyrrole/graphene composite material and 1. to magnify, Ma Yanwei, open " a kind of preparation method of polypyrrole/graphene composite material " the Chinese patent CN101882480A of bear, Chen Yao and Yu Peng and 2. " polypyrrole/graphene nano composite material and preparation thereof " Chinese patent CN102051048A of honor reason, Gao Qian, Guo Ruibin, Liu Pengwei, Zhao Yongxia and Feng Chao not.In above-mentioned patent 1.; Chemical polymerization is adopted in the preparation of polypyrrole/graphene; The product of graphite oxide after through hydrazine hydrate reduction obtained homodisperse Graphene colloid with deionized water wash; Mix the ultrasonic dispersion in back according to a certain percentage with this colloid and pyrrole monomer, place condition of ice bath to stir then, again with FeCl
3Hydrochloric acid solution add in the reactant and accomplish.In patent 2., adopt situ aggregation method, be medium with ethanol, with the p-methyl benzenesulfonic acid surfactant, with polyethylene glycol-400 phase transfer catalyst, with FeCl
36H
2O is an initator, and the pyrrole monomer in-situ polymerization is got final product on Graphene.
In the document and patent of these preparation polypyrrole/graphene composite materials, adopt chemical method basically, prepared polypyrrole microstructure is membranaceous or sheet; The form with nano wire does not exist; Conductivity own is not very high, and the adding of Graphene has improved the polypyrrole performance to a certain extent, but because the end product of compound is a powder; Be difficult to fix, on using, be restricted.
Summary of the invention
Technology contents:The present invention seeks to overcome that there is the not high shortcoming of conductivity simultaneously in end product with powder type in the existing polypyrrole/graphene composite material preparation, propose a kind of method for preparing polypyrrole nano line/graphene composite material.The present invention is an electrolyte with sodium hydrogen phosphate and lithium perchlorate, adopts electrochemical production polypyrrole nano line/graphene composite material.Technology of the present invention is simple, the time is short, operating process is controlled, with low cost; The 1-dimention nano line structure of the composite material of preparation has improved specific area greatly; Conductivity is high; Can directly be fixed as electrode, it can be used as electrode material and is applied in fuel cell, can also be applied in aspects such as ultracapacitor, lithium battery, transducer.
Technical scheme:The step of preparation process order that the present invention prepares polypyrrole nano line-graphene composite material method is as follows:
1) is electrolyte with sodium hydrogen phosphate and lithium perchlorate, is configured to electrolyte;
2) in above-mentioned sodium hydrogen phosphate and lithium perchlorate mixed electrolytic solution, add pyrrole monomer, through stirring; Add graphene powder then, under the ultrasonic wave effect, form homodisperse mixed solution;
3) adopt the electrochemical method polymerization, polymerization obtains polypyrrole nano line/graphene composite material sample on conductive substrates; The gained sample is dried after washing with ethanol, distilled water respectively.
Sodium hydrogen phosphate concentration in said preparation method's the step 1) is 0.1mol/L-0.3mol/L, and lithium perchlorate concentration is 0.001mol/L-0.01mol/L.
The concentration range of the pyrrole monomer said preparation method's step 2) is 0.1mol/L-0.3mol/L.
Said preparation method's step 2) pyrrole monomer in and the mass percent of graphene powder are 95%-60%:5%-40%.
Electrochemical method in said preparation method's the step 3) is a constant-voltage method, and the polymerization voltage range of constant-voltage method is 0.7V-1.8V.
Conductive substrates in said preparation method's the step 3) is the inert metal electrode that sheet, bulk or form of film exist, and can also be carbon-based material.
Said inert metal is: nickel, zinc, copper, stainless steel, silver, gold.
Said carbon-based material is: carbon paper, carbon cloth, carbon felt, carbon-point, reticulated vitreous carbon fiber, active carbon, graphite felt, graphite flake, graphite rod or foamy graphite.
Polymerization time in the step 3) of prepared method is 0.5min-60min.
Beneficial effect:Technology of the present invention is simple, the time is short, operating process is controlled, with low cost; The composite material conductivity of preparation is high; Can directly be fixed as electrode, can be used as electrode material and be applied in fuel cell, can also be applied in aspects such as ultracapacitor, lithium battery, transducer.
Description of drawings
Fig. 1 is the sem photograph of the polypyrrole nano line/graphene composite material of the embodiment of the invention 1;
Fig. 2 is that the nickel sheet substrate that covers of the polypyrrole nano line/graphene composite material of the embodiment of the invention 1 is at 0.2M LiClO
4Cyclic voltammetry curve in the solution;
Fig. 3 is that the nickel sheet substrate that covers of the polypyrrole nano line/graphene composite material of the embodiment of the invention 1 is at 0.2M LiClO
4Electrochemical impedance spectral curve in the solution;
Fig. 4 is that the nickel sheet substrate that covers of the polypyrrole nano line/graphene composite material of the embodiment of the invention 2 is at 0.2M LiClO
4Cyclic voltammetry curve in the solution;
Fig. 5 is that the nickel sheet substrate that covers of the polypyrrole nano line/graphene composite material of the embodiment of the invention 2 is at 0.2M LiClO
4Electrochemical impedance spectral curve in the solution;
Fig. 6 is that the nickel sheet substrate that covers of the polypyrrole nano line/graphene composite material of the embodiment of the invention 3 is at 0.2M LiClO
4Cyclic voltammetry curve in the solution;
Fig. 7 is that the nickel sheet substrate that covers of the polypyrrole nano line/graphene composite material of the embodiment of the invention 3 is at 0.2M LiClO
4Electrochemical impedance spectral curve in the solution;
Fig. 8 is that the carbon cloth substrate that covers of the polypyrrole nano line/graphene composite material of the embodiment of the invention 4 is at 0.2M LiClO
4Electrochemical impedance spectral curve in the solution;
Fig. 9 is that the carbon cloth substrate that covers of the polypyrrole nano line/graphene composite material of the embodiment of the invention 4 is at 0.2M LiClO
4Electrochemical impedance spectral curve in the solution.
Embodiment
1) be electrolyte with sodium hydrogen phosphate and lithium perchlorate, sodium hydrogen phosphate concentration is 0.1mol/L-0.3mol/L, and lithium perchlorate concentration is 0.001mol/L-0.01mol/L, and is even with magnetic stirrer.
2) in above-mentioned sodium hydrogen phosphate and lithium perchlorate electrolyte, add pyrrole monomer, through stirring; The graphene powder that adds certain mass then under ultrasonication, forms homodisperse mixed solution.The concentration range of the pyrrole monomer among the said preparation method is 0.1mol/L-0.3mol/L, and the mass percent of pyrrole monomer and graphene powder is 95%:5%-60%:40%.
3) constant-voltage method in the employing electrochemical method, behind the polymerase 10 .5min-60min, polymerization obtains polypyrrole nano line/graphene composite material sample on conductive substrates; The gained sample is dried after washing with ethanol, distilled water respectively.Conductive substrates among the described preparation method is the inert metal electrode that exists with multi-form (like sheet, bulk, form of film etc.); Like nickel, zinc, copper, stainless steel, silver, gold etc.; Also can be the carbon-based material that exists with multi-form, like carbon paper, carbon cloth, carbon felt, carbon-point, reticulated vitreous carbon fiber, active carbon, graphite felt, graphite flake (rod), foamy graphite etc.
Embodiment 1
(1) configuration electrolyte: take by weighing 3.08g sodium hydrogen phosphate and 0.08g lithium perchlorate, add the 50ml deionized water, be configured as the mixed electrolytic solution that contains 0.2M sodium hydrogen phosphate and 0.01M lithium perchlorate, use magnetic stirrer 30min.Mass percent according to pyrroles and Graphene is the ratio proportioning of 90%:10%, takes by weighing 0.5g (0.075M) pyrrole monomer and adds in the electrolyte magnetic agitation 10min.
(2) preparation polypyrrole nano line/graphene composite material: in the above-mentioned solution, add the 0.06g Graphene, leave standstill behind the ultrasonic 30min and obtain homodisperse mixed solution.Polymerization experiment is carried out in the three-electrode system of electrochemical workstation control, is work electrode with the nickel sheet, and platinized platinum is to electrode, and saturated calomel electrode is a reference electrode.Use potentiostatic method, polymerization voltage is 0.8V, and resulting sample dries after washing with ethanol, deionization.
(3) the cyclic voltammetric characteristic test of polypyrrole nano line/graphene composite material: the LiClO of configuration 0.2M
4Solution 50ml in the three-electrode system of electrochemical workstation control, uses cyclic voltammetry, and the setting voltage parameter area is-0.9V-0.9V that sweep speed is 50mV/s, tests.
(4) the electrochemical impedance performance test of polypyrrole nano line/graphene composite material: the LiClO of configuration 0.2M
4Solution 50ml, with electrode of preparation in (2) be placed on soak 30min in the solution after, in the three-electrode system of electrochemical workstation control; Select the electrochemical impedance spectrometry, the starting voltage parameter is made as 0V, and range of scanned frequencies is made as 0.01Hz-100KHz; Signal amplitude is made as 5mV, tests.
Embodiment 2
(1) configuration electrolyte: take by weighing 3.08g sodium hydrogen phosphate and 0.08g lithium perchlorate, add the 50ml deionized water, be configured to contain the mixed electrolytic solution of 0.2M sodium hydrogen phosphate and 0.01M lithium perchlorate, use magnetic stirrer 30min.Mass percent according to pyrroles and Graphene is the ratio proportioning of 60%:40%, takes by weighing 0.5g (0.075M) pyrrole monomer and adds in the electrolyte magnetic agitation 10min.
(2) preparation polypyrrole nano line/graphene composite material: in the above-mentioned solution, add the 0.34g Graphene, leave standstill behind the ultrasonic 30min and obtain homodisperse mixed solution.Polymerization experiment is carried out in the three-electrode system of electrochemical workstation control, is work electrode with the nickel sheet, and platinized platinum is to electrode, and saturated calomel electrode is a reference electrode.Use potentiostatic method, polymerization voltage is 0.8V, and resulting sample dries after washing with ethanol, deionization.
(3) the cyclic voltammetric characteristic test of polypyrrole nano line/graphene composite material: the LiClO of configuration 0.2M
4Solution 50ml in the three-electrode system of electrochemical workstation control, uses cyclic voltammetry, and the setting voltage parameter area is-1.0V-1.0V that sweep speed is 50mV/s, tests.
(4) the electrochemical impedance performance test of polypyrrole nano line/graphene composite material: the LiClO of configuration 0.2M
4Solution 50ml, with electrode of preparation in (2) be placed on soak 30min in the solution after, in the three-electrode system of electrochemical workstation control; Select the electrochemical impedance spectrometry, the starting voltage parameter is made as 0V, and range of scanned frequencies is made as 0.01Hz-100KHz; Signal amplitude is made as 5mV, tests.
Embodiment 3
(1) configuration electrolyte: take by weighing 3.08g sodium hydrogen phosphate and 0.08g lithium perchlorate, add the 50ml deionized water, be configured to contain the mixed electrolytic solution of 0.2M sodium hydrogen phosphate and 0.01M lithium perchlorate, use magnetic stirrer 30min.Mass percent according to pyrroles and Graphene is the ratio proportioning of 80%:20%, in electrolyte, adds 0.85g (0.125M) pyrrole monomer, magnetic agitation 10min.
(2) preparation polypyrrole nano line/graphene composite material: take by weighing the 0.21g Graphene and add in the above-mentioned solution, leave standstill behind the ultrasonic 30min and obtain homodisperse mixed solution.Polymerization experiment is carried out in the three-electrode system of electrochemical workstation control, is work electrode with the nickel sheet, and platinized platinum is to electrode, and saturated calomel electrode is a reference electrode.Use potentiostatic method, polymerization voltage is 0.8V, and resulting sample dries after washing with ethanol, deionization.
(3) the cyclic voltammetric characteristic test of polypyrrole nano line/graphene composite material: the LiClO of configuration 0.2M
4Solution 50ml in the three-electrode system of electrochemical workstation control, uses cyclic voltammetry, and the setting voltage parameter area is-1.0V-1.0V that sweep speed is 50mV/s, tests.
(4) the electrochemical impedance performance test of polypyrrole nano line/graphene composite material: the LiClO of configuration 0.2M
4Solution 50ml, with electrode of preparation in (2) be placed on soak 30min in the solution after, in the three-electrode system of electrochemical workstation control; Select the electrochemical impedance spectrometry, the starting voltage parameter is made as 0V, and range of scanned frequencies is made as 0.01Hz-100KHz; Signal amplitude is made as 5mV, tests.
(1) configuration electrolyte: take by weighing 3.08g sodium hydrogen phosphate and 0.08g lithium perchlorate, add the 50ml deionized water, be configured as the mixed electrolytic solution that contains 0.2M sodium hydrogen phosphate and 0.01M lithium perchlorate, use magnetic stirrer 30min.Mass percent according to pyrroles and Graphene is the ratio proportioning of 80%:20%, takes by weighing 0.5g (0.075M) pyrrole monomer and adds in the electrolyte magnetic agitation 10min.
(2) preparation polypyrrole nano line/graphene composite material: in the above-mentioned solution, add the 0.13g Graphene, leave standstill behind the ultrasonic 30min and obtain homodisperse mixed solution.Polymerization experiment is carried out in the three-electrode system of electrochemical workstation control, is work electrode with the carbon cloth, and platinized platinum is to electrode, and saturated calomel electrode is a reference electrode.Use potentiostatic method, polymerization voltage is 0.8V, and resulting sample dries after washing with ethanol, deionization.
(3) the cyclic voltammetric characteristic test of polypyrrole nano line/graphene composite material: the LiClO of configuration 0.2M
4Solution 50ml in the three-electrode system of electrochemical workstation control, uses cyclic voltammetry, and the setting voltage parameter area is-0.9V-0.9V that sweep speed is 50mV/s, tests.
(4) the electrochemical impedance performance test of polypyrrole nano line/graphene composite material: the LiClO of configuration 0.2M
4Solution 50ml, with electrode of preparation in (2) be placed on soak 30min in the solution after, in the three-electrode system of electrochemical workstation control; Select the electrochemical impedance spectrometry, the starting voltage parameter is made as 0V, and range of scanned frequencies is made as 0.01Hz-100KHz; Signal amplitude is made as 5mV, tests.
Claims (9)
1. method for preparing polypyrrole nano line-graphene composite material is characterized in that this preparation method's sequence of process steps is following:
1) is electrolyte with sodium hydrogen phosphate and lithium perchlorate, is configured to electrolyte;
2) in above-mentioned sodium hydrogen phosphate and lithium perchlorate mixed electrolytic solution, add pyrrole monomer, through stirring; Add graphene powder then, under the ultrasonic wave effect, form homodisperse mixed solution;
3) adopt the electrochemical method polymerization, polymerization obtains polypyrrole nano line/graphene composite material sample on conductive substrates; The gained sample is dried after washing with ethanol, distilled water respectively.
2. the preparation method of polypyrrole nano line-graphene composite material according to claim 1; It is characterized in that: the sodium hydrogen phosphate concentration in said preparation method's the step 1) is 0.1mol/L-0.3mol/L, and lithium perchlorate concentration is 0.001mol/L-0.01mol/L.
3. the preparation method of polypyrrole nano line-graphene composite material according to claim 1, it is characterized in that: the concentration range of the pyrrole monomer said preparation method's step 2) is 0.1mol/L-0.3mol/L.
4. the preparation method of polypyrrole nano line-graphene composite material according to claim 1, it is characterized in that: the pyrrole monomer said preparation method's step 2) and the mass percent of graphene powder are 95%-60%:5%-40%.
5. the preparation method of polypyrrole nano line-graphene composite material according to claim 1, it is characterized in that: the electrochemical method in said preparation method's the step 3) is a constant-voltage method, the polymerization voltage range of constant-voltage method is 0.7V-1.8V.
6. the preparation method of polypyrrole nano line-graphene composite material according to claim 1; It is characterized in that: the conductive substrates in said preparation method's the step 3) is the inert metal electrode that sheet, bulk or form of film exist, and can also be the carbon-based material that exists with multi-form.
7. the preparation method of polypyrrole nano line-graphene composite material according to claim 6, it is characterized in that: said inert metal is: nickel, zinc, copper, stainless steel, silver, gold.
8. the preparation method of polypyrrole nano line-graphene composite material according to claim 6, it is characterized in that: said carbon-based material is: carbon paper, carbon cloth, carbon felt, carbon-point, reticulated vitreous carbon fiber, active carbon, graphite felt, graphite flake, graphite rod or foamy graphite.
9. the preparation method of polypyrrole nano line-graphene composite material according to claim 1, it is characterized in that: the polymerization time in the step 3) of prepared method is 0.5min-60min.
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