CN103413695A - Macroscopic-quantity preparation method for macroscopic three-dimensional graphene/tin oxide composite material - Google Patents
Macroscopic-quantity preparation method for macroscopic three-dimensional graphene/tin oxide composite material Download PDFInfo
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- CN103413695A CN103413695A CN2013103040097A CN201310304009A CN103413695A CN 103413695 A CN103413695 A CN 103413695A CN 2013103040097 A CN2013103040097 A CN 2013103040097A CN 201310304009 A CN201310304009 A CN 201310304009A CN 103413695 A CN103413695 A CN 103413695A
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Abstract
The invention discloses a macroscopic-quantity preparation method for macroscopic three-dimensional graphene/tin oxide composite material. According to the preparation method, stannous chloride and hydrochloric acid are added into graphene oxide suspension liquid, and after reaction, a macroscopic three-dimensional graphene/tin oxide composite material hydrogel is obtained; after deionized water is used for washing and freeze-drying is performed, a macroscopic three-dimensional graphene/tin oxide composite material aerogel is obtained. The macroscopic three-dimensional graphene/tin oxide composite material aerogel is prepared for the first time, and the synthetic method has the advantages of being low in cost, green, environmentally friendly, simple, easy to operate and control and capable of preparing in a macroscopic-quantity mode. The macroscopic-quantity preparation method is suitable for industrialized large-scale production. The problem that SnO2 serves as electrodes of a pseudo capacitance super capacitor and is low in power density due to the poor electrical conductivity is solved. Graphene flakes are assembled to form a three-dimensional macrostructure, and therefore the problem that according to a common method, in the preparation process of graphene-based super capacitor material, due to the aggregation of the graphene, application performance is degraded sharply is solved.
Description
Technical field
The invention belongs to the preparing technical field of the C-base composte material that can be used for energy storage device, relate to the preparation in macroscopic quantity method of a kind of macroscopical three-dimensional grapheme that can be used for ultracapacitor/tin oxide composite material aeroge.
Background technology
Ultracapacitor is a kind of novel energy-storing element between conventional electrostatic capacitor and battery.With the conventional electrostatic capacitor, compare, ultracapacitor has higher energy density; With battery, compare, ultracapacitor has higher power density.Ultracapacitor also has and has extended cycle life, discharges and recharges the advantage such as speed is fast.In fields such as mobile communication, consumer electronics, electric automobile, Aero-Space and national defence, boundless application prospect is arranged.At present the research of ultracapacitor caused to very big concern at world wide.By the energy storage principle ultracapacitor, usually be divided into fake capacitance ultracapacitor and double electric layers supercapacitor.The fake capacitance ultracapacitor is mainly to utilize at electrode surface or the quick and reversible redox reaction of near surface generation to realize energy storage, and the electrode material of fake capacitance ultracapacitor is mainly transition metal oxide (as SnO
2, MnO
2Deng) and conducting polymer (as polyaniline, polypyrrole etc.).Double electric layers supercapacitor is to utilize positive and negative ion absorption respectively on the interface between two electrodes and electrolyte, cause two electrical potential differences between electrode to realize energy storage, double electric layers supercapacitor usually adopts and has the carbon back active material of high-specific surface area as electrode material.
SnO
2Electrode material as the fake capacitance ultracapacitor shows very high energy density, but because the shortcoming of its poorly conductive causes its power density very low.Compound with the carbon nanomaterial of good conductivity is to address this problem good approach.In dissimilar carbon nanomaterial, Graphene, due to the conductivity with very large specific area, excellence, in advantages such as the medium-altitude stability of electrochemical environment, is suitable as the electrode material of double electric layers supercapacitor very much.But because making it, strong intermolecular force between the very strong hydrophobicity of graphene sheet layer and lamella is very easy to reunite, the result of reuniting causes the specific area of Graphene sharply to descend, and has a strong impact on the performance of Graphene as the double electric layers supercapacitor electrode material.It is to address this problem extraordinary approach that graphene sheet layer is prepared into to macroscopical three-dimensional aeroge by the method for assembling.If introduce us and can predict and can prepare a kind of macroscopical three-dimensional grapheme/tin oxide composite material aeroge by top, this material will be suitable as the electrode material of ultracapacitor very much.But up to the present, also there is no this Graphene of a kind of method energy preparation in macroscopic quantity/tin oxide composite material aeroge.
Summary of the invention
The object of the invention is to come preparation in macroscopic quantity to can be used for the present situation of macroscopical three-dimensional grapheme of ultracapacitor/tin oxide composite material aeroge for current shortage simple effective method, utilize graphite oxide, stannous chloride and hydrochloric acid to be raw material, provide a kind of simple to operate, productive rate is high, the preparation in macroscopic quantity method of macroscopical three-dimensional grapheme of environmental protection/tin oxide composite material aeroge.Described preparation method comprises the steps:
The first step, prepare graphite oxide by classical hummer method;
Second step, be distributed to dialysis in water by the graphite oxide of preparation and fully, remove metal ion and acid remaining in graphite oxide;
The 3rd step, by the ultrasonic processing of solution after dialysis, then centrifugation, the suspension of acquisition graphene oxide, then obtain by dilution the graphene oxide suspension that concentration is 2mg/ml;
The 4th step, get graphene oxide suspension 15-100ml, then adds stannous chloride and hydrochloric acid, forms mixed solution.In mixed solution, the concentration of stannous chloride is respectively 0.004～0.01M, and the concentration of hydrochloric acid is 0.08～0.2M, reacts 15～60 minutes under 90 ℃ of conditions that do not stir, and has finally obtained macroscopical three-dimensional grapheme/tin oxide composite material hydrogel;
The 5th step, the composite material hydrogel of acquisition is washed to remove remaining impurity with deionized water, then utilizing the method for freeze-drying, is subzero 45 ℃ in temperature, and pressure is that under the condition of 0.02mbar, freeze-drying obtained macroscopical Graphene/tin oxide composite material aeroge in 72～96 hours.
In the present invention, if not explanation especially, all prepared by the solution adopted, such as what at room temperature substance dissolves is prepared in the aqueous solution under normal condition.
In the present invention, if not explanation especially, the device adopted, instrument, equipment, material, technique, method, step, preparation condition etc. are all that this area routine adopts or those of ordinary skills can easily obtain according to the conventional technology adopted in this area.
Than the existing method for preparing three-dimensional grapheme based composites aeroge, the present invention has following advantage:
1, the present invention has prepared macroscopical three-dimensional grapheme/tin oxide composite material aeroge first.Adopt gentle solwution method, but synthetic method has that cost is low, environmental protection, simple, be easy to control the advantage such as preparation in macroscopic quantity, be applicable to industrial mass production;
2, compound by the Graphene with having the superior electrical conductivity energy, solved SnO
2As the electrode of fake capacitance ultracapacitor because its poorly conductive causes the problem that its power density is low.Because graphene film in preparation process has formed the three-dimensional macro structure by assembling, solved conventional method causes its application performance sharply to descend due to the reunion of Graphene in the process of the graphene-based super capacitor material of preparation problem.Prepared macroscopical three-dimensional grapheme/tin oxide composite material aeroge will be extraordinary electrode material for super capacitor.
The accompanying drawing explanation
Fig. 1 is the photo of the prepared Graphene of the embodiment of the present invention 1/tin oxide composite material aeroge.
Fig. 2 is the stereoscan photograph of the prepared Graphene of the embodiment of the present invention 1/tin oxide composite material aeroge.
Fig. 3 is the photo of the prepared bulk Graphene of the embodiment of the present invention 2/tin oxide composite material aeroge.
Embodiment
Below in conjunction with drawings and Examples, specifically describe the preparation in macroscopic quantity method of macroscopical three-dimensional grapheme of the present invention/tin oxide composite material aeroge; but be to be understood that; these embodiment are only be used to setting forth the present invention, and and limit the scope of the invention never in any form.
Adopt preparation in macroscopic quantity method provided by the invention to prepare macroscopical three-dimensional grapheme/tin oxide composite material aeroge, concrete steps are as follows:
The first step, prepare graphite oxide by classical hummer method;
Second step, be distributed to dialysis in water by the graphite oxide of preparation and fully, remove metal ion and acid remaining in graphite oxide;
The 3rd step, by the ultrasonic processing of solution after dialysis, then centrifugation, the suspension of acquisition graphene oxide, obtain by dilution the graphene oxide suspension that concentration is 2mg/ml;
The 4th step, get graphene oxide suspension 15ml, then adds stannous chloride and hydrochloric acid, forms mixed solution.In mixed solution, the concentration of stannous chloride is respectively 0.004M, and the concentration of hydrochloric acid is 0.08M, and reaction is 60 minutes under 90 ℃ of conditions that do not stir, and finally obtains macroscopical three-dimensional grapheme/tin oxide composite material hydrogel;
The 5th step, macroscopical three-dimensional grapheme of acquisition/tin oxide composite material hydrogel is washed to remove remaining impurity with deionized water, then utilize the method for freeze-drying, in temperature, be subzero 45 ℃, pressure is that under the condition of 0.02mbar, freeze-drying obtained macroscopical Graphene/tin oxide composite material aeroge in 72 hours.Photo such as Fig. 1 of the composite material aeroge prepared, Fig. 1 show that prepared composite material is macroscopical three-dimensional whole block material.Fig. 2 is the stereoscan photograph of composite material aeroge, the internal structure of bulk product is the three-dimensional aeroge assembled by graphene sheet layer as seen from Figure 2, the graphene sheet layer that forms aeroge is very thin, has solved from graphene oxide and has prepared the problem that the general graphene sheet layer of Graphene is easily reunited.
Adopt method provided by the invention to prepare macroscopical three-dimensional grapheme/tin oxide composite material, concrete steps are as follows:
The first step, prepare graphite oxide by classical hummer method;
Second step, be distributed to dialysis in water by the graphite oxide of preparation and fully, remove metal ion and acid remaining in graphite oxide;
The 3rd step, by the ultrasonic processing of solution after dialysis, then centrifugation, the suspension of acquisition graphene oxide; By dilution, obtain the graphene oxide suspension that concentration is 2mg/ml;
The 4th step, get graphene oxide suspension 100ml, then add stannous chloride and hydrochloric acid, in mixed solution, the concentration of stannous chloride is respectively 0.004M, the concentration of hydrochloric acid is 0.08M, reaction is 60 minutes under 90 ℃ of conditions that do not stir, and has finally obtained macroscopical three-dimensional grapheme/tin oxide composite material hydrogel;
The 5th step, by obtaining the composite material hydrogel, wash to remove remaining unnecessary impurity with deionized water, then utilizing the method for freeze-drying, is subzero 45 ℃ in temperature, and pressure is that under the condition of 0.02mbar, freeze-drying obtained macroscopical Graphene/tin oxide composite material aeroge in 72 hours.Photo such as Fig. 3 of the composite material aeroge prepared, Fig. 3 show that prepared composite material is macroscopical three-dimensional bulk integral material.With embodiment 1, compare, by increasing the volume ratio of graphene oxide suspension, can preparation in macroscopic quantity bulk Graphene/tin oxide composite material aeroge, the diameter of the cylindric aeroge that embodiment 1 forms is about 1.5cm, and in this example, the diameter of aeroge is about 5.5cm.
Embodiment 3
Adopt method provided by the invention to prepare macroscopical three-dimensional grapheme/tin oxide composite material, concrete steps are as follows:
The first step, prepare graphite oxide by classical hummer method;
Second step, be distributed to dialysis in water by the graphite oxide of preparation and fully, remove metal ion and acid remaining in graphite oxide;
The 3rd step, by the ultrasonic processing of solution after dialysis, then centrifugation, the suspension of acquisition graphene oxide; By dilution, obtain the graphene oxide suspension that concentration is 2mg/ml;
The 4th step, get graphene oxide suspension 15ml, then add stannous chloride and hydrochloric acid, in mixed solution, the concentration of stannous chloride is respectively 0.004M, the concentration of hydrochloric acid is 0.08M, reaction is 15 minutes under 90 ℃ of conditions that do not stir, and has finally obtained macroscopical three-dimensional grapheme/tin oxide composite material hydrogel;
The 5th step, by obtaining the composite material hydrogel, wash to remove remaining unnecessary impurity with deionized water, then utilizing the method for freeze-drying, is subzero 45 ℃ in temperature, and pressure is that under the condition of 0.02mbar, freeze-drying obtained macroscopical Graphene/tin oxide composite material aeroge in 72 hours.
Embodiment 4
The first step, prepare graphite oxide by classical hummer method;
Second step, be distributed to dialysis in water by the graphite oxide of preparation and fully, remove metal ion and acid remaining in graphite oxide;
The 3rd step, by the ultrasonic processing of solution after dialysis, then centrifugation, the suspension of acquisition graphene oxide; By dilution, obtain the graphene oxide suspension that concentration is 2mg/ml;
The 4th step, get graphene oxide suspension 15ml, then add stannous chloride and hydrochloric acid, in mixed solution, the concentration of stannous chloride is respectively 0.004M, the concentration of hydrochloric acid is 0.08M, reaction is 30 minutes under 90 ℃ of conditions that do not stir, and has finally obtained macroscopical three-dimensional grapheme/tin oxide composite material hydrogel;
The 5th step, by obtaining the composite material hydrogel, wash to remove remaining unnecessary impurity with deionized water, then utilizing the method for freeze-drying, is subzero 45 ℃ in temperature, and pressure is that under the condition of 0.02mbar, freeze-drying obtained macroscopical Graphene/tin oxide composite material aeroge in 72 hours.
Embodiment 5
The first step, prepare graphite oxide by classical hummer method;
Second step, be distributed to dialysis in water by the graphite oxide of preparation and fully, remove metal ion and acid remaining in graphite oxide;
The 3rd step, by the ultrasonic processing of solution after dialysis, then centrifugation, the suspension of acquisition graphene oxide; By dilution, obtain the graphene oxide suspension that concentration is 2mg/ml;
The 4th step, get graphene oxide suspension 50ml, then add stannous chloride and hydrochloric acid, in mixed solution, the concentration of stannous chloride is respectively 0.01M, the concentration of hydrochloric acid is 0.2M, reaction is 60 minutes under 90 ℃ of conditions that do not stir, and has finally obtained macroscopical three-dimensional grapheme/tin oxide composite material hydrogel;
The 5th step, by obtaining the composite material hydrogel, wash to remove remaining unnecessary impurity with deionized water, then utilizing the method for freeze-drying, is subzero 45 ℃ in temperature, and pressure is that under the condition of 0.02mbar, freeze-drying obtained macroscopical Graphene/tin oxide composite material aeroge in 96 hours.
Embodiment 6
The first step, prepare graphite oxide by classical hummer method;
Second step, be distributed to dialysis in water by the graphite oxide of preparation and fully, remove metal ion and acid remaining in graphite oxide;
The 3rd step, by the ultrasonic processing of solution after dialysis, then centrifugation, the suspension of acquisition graphene oxide; Method acquisition concentration by dilution is the graphene oxide suspension of 2mg/ml;
The 4th step, get graphene oxide suspension 100ml, then add stannous chloride and hydrochloric acid, in mixed solution, the concentration of stannous chloride is respectively 0.006M, the concentration of hydrochloric acid is 0.1M, reaction is 60 minutes under 90 ℃ of conditions that do not stir, and has finally obtained macroscopical three-dimensional grapheme/tin oxide composite material hydrogel;
The 5th step, by obtaining the composite material hydrogel, wash to remove remaining unnecessary impurity with deionized water, then utilizing the method for freeze-drying, is subzero 45 ℃ in temperature, and pressure is that under the condition of 0.02mbar, freeze-drying obtained macroscopical Graphene/tin oxide composite material aeroge in 96 hours.
The Graphene that above-described embodiment prepares/tin oxide composite material aeroge is macroscopical three-dimensional structure, and the size of composite material aeroge is between 1.5-5.5cm.
Claims (4)
1. the preparation in macroscopic quantity method of macroscopical three-dimensional grapheme/tin oxide composite material aeroge, is characterized in that, comprises the steps:
The first step, prepare graphite oxide by classical hummer method;
Second step, be distributed to dialysis in water by the graphite oxide of preparation and fully, remove metal ion and acid remaining in graphite oxide;
The 3rd step, by the ultrasonic processing of solution after dialysis, then centrifugation, the suspension of acquisition graphene oxide, then obtain by dilution the graphene oxide suspension that concentration is 2mg/ml;
The 4th step, get graphene oxide suspension 15～100ml, then adds stannous chloride and hydrochloric acid, forms mixed solution; In mixed solution, the concentration of stannous chloride is respectively 0.004～0.01M, and the concentration of hydrochloric acid is 0.08～0.2M, reacts 15～60 minutes under 90 ℃ of conditions that do not stir, and has finally obtained macroscopical three-dimensional grapheme/tin oxide composite material hydrogel;
The 5th step, wash the composite material hydrogel of acquisition with deionized water, then utilize the method for freeze-drying, is subzero 45 ℃ in temperature, and pressure is that under the condition of 0.02mbar, freeze-drying obtained macroscopical Graphene/tin oxide composite material aeroge in 72～96 hours.
2. macroscopical three-dimensional grapheme/tin oxide composite material aeroge, is characterized in that: adopt method claimed in claim 1 to prepare; Prepared composite material aeroge is macroscopical three-dimensional structure, and internal structure is the three-dimensional aeroge assembled by graphene sheet layer.
3. macroscopical three-dimensional grapheme according to claim 2/tin oxide composite material aeroge, it is characterized in that: the diameter of described aeroge is 1.5cm～5.5cm.
4. the application of macroscopical three-dimensional grapheme/tin oxide composite material aeroge is characterized in that: described composite material aeroge is for the preparation of the C-base composte material of energy storage device.
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Cited By (6)
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| CN105826541A (en) * | 2016-06-14 | 2016-08-03 | 中科探能（北京）科技有限公司 | Graphene-doped stannic-oxide-based lithium nano battery cathode material and preparation method |
| CN106683902A (en) * | 2016-12-29 | 2017-05-17 | 铜陵市胜美达电子制造有限公司 | High-specific-capacity cobaltosic oxide nanowire carbon aerogel hybrid supercapacitor anode material and preparation method thereof |
| CN106744812A (en) * | 2017-02-21 | 2017-05-31 | 中国林业科学研究院木材工业研究所 | A kind of compound carbon aerogels and preparation method thereof |
| CN108940140A (en) * | 2018-07-20 | 2018-12-07 | 北京欧美中科学技术研究院 | A method of preparing graphene carbon aerogel composite |
| CN109524170A (en) * | 2018-10-30 | 2019-03-26 | 天津市职业大学 | A kind of preparation method of graphene and fluorin-doped tin oxide transparent conductive film |
| CN109775748A (en) * | 2019-03-07 | 2019-05-21 | 南京工业大学 | A kind of SnO with gas-sensitive property2The preparation method of graphene aerogel material |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105826541A (en) * | 2016-06-14 | 2016-08-03 | 中科探能（北京）科技有限公司 | Graphene-doped stannic-oxide-based lithium nano battery cathode material and preparation method |
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| CN106683902A (en) * | 2016-12-29 | 2017-05-17 | 铜陵市胜美达电子制造有限公司 | High-specific-capacity cobaltosic oxide nanowire carbon aerogel hybrid supercapacitor anode material and preparation method thereof |
| CN106744812A (en) * | 2017-02-21 | 2017-05-31 | 中国林业科学研究院木材工业研究所 | A kind of compound carbon aerogels and preparation method thereof |
| CN106744812B (en) * | 2017-02-21 | 2019-02-22 | 中国林业科学研究院木材工业研究所 | A kind of compound carbon aerogels and preparation method thereof |
| CN108940140A (en) * | 2018-07-20 | 2018-12-07 | 北京欧美中科学技术研究院 | A method of preparing graphene carbon aerogel composite |
| CN108940140B (en) * | 2018-07-20 | 2020-06-30 | 北京欧美中科学技术研究院 | Method for preparing graphene carbon aerogel composite material |
| CN109524170A (en) * | 2018-10-30 | 2019-03-26 | 天津市职业大学 | A kind of preparation method of graphene and fluorin-doped tin oxide transparent conductive film |
| CN109775748A (en) * | 2019-03-07 | 2019-05-21 | 南京工业大学 | A kind of SnO with gas-sensitive property2The preparation method of graphene aerogel material |
| CN109775748B (en) * | 2019-03-07 | 2021-06-22 | 南京工业大学 | SnO with gas-sensitive characteristic2Preparation method of-graphene aerogel material |
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Application publication date: 20131127 |