CN106744841A - A kind of preparation method of the three-dimensional porous graphene film that single-layer graphene is constructed - Google Patents
A kind of preparation method of the three-dimensional porous graphene film that single-layer graphene is constructed Download PDFInfo
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
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Abstract
A kind of preparation method and application of the three-dimensional grapheme film that utilization single-layer graphene is constructed.It is characterized in that：Ultrasonic Pulverization and ball milling stripping technology are added in the improvement Hummer method technical process for prepare Graphene, obtain the Graphene of individual layer or few layer, Graphene slurry is mixed with out with organic solvent, the Graphene slurry of different-thickness is printed in substrate in the method for silk-screen printing, this substrate for being printed with Graphene slurry is placed in Muffle furnace, to obtain a kind of interconnection, the graphene film with nano level porous three-dimensional structure after the method removal organic ink of high-temperature heat treatment.The film has high-specific surface area, as electrode materials such as ultracapacitor, lithium ion battery, thin-film solar cells after being modified using metal oxide, metal sulfide.
Description
Technical field
The present invention relates to Material Field, and in particular to a kind of system of the three-dimensional grapheme film that utilization single-layer graphene is constructed
Preparation Method and application.
Background technology
Graphene is a kind of material of the individual layer laminated structure being made up of carbon atom, is led with specific surface area and height higher
Electric rate and splendid mechanical performance, hence in so that the material based on Graphene turns into extremely promising energy storage active material,
Especially as the electrode material of double electric layers supercapacitor.
However, the hydrophobic property of the stronger Van der Waals force of graphene nanometer sheet interlayer and Graphene causes graphene sheet layer
Easily layer upon layer, how the graphene-based sorbing material of synthesized high-performance is key in graphene-based sorbing material research is asked
Topic, it is a kind of very effective method to construct graphene-based porous three-dimensional frame structure.Compare original graphite alkene and other forms
The graphene-based material of structure, based on its three-dimensional network and loose structure feature, the graphene-based material list of three-dimensional frame structure
Reveal more excellent physicochemical properties.Three-dimensional grapheme material, is structurally different from the Graphene of two dimension, and it is effective
Overcome two-dimensional graphene easily to reunite, hardly possible dispersion, it is difficult to obtain the shortcoming of high-specific surface area, this causes that it is more suitable for double electricity
The electrode material of layer ultracapacitor.Three-dimensional grapheme has three-dimensional hollow porous network structure, and net wall is Graphene, is stratiform
The graphite of structure and porous graphitic carbon foam, with ultralow close DEG C of surface area, high heat conduction, high temperature resistant, corrosion-resistant, extension
Property, the advantages of pliability is good.
The preparation method of Graphene mainly has：Physical method, mechanical stripping method, chemical vapour deposition technique, thermal expansion is peeled off
Method, electrochemical process, oxidation-reduction method etc..Chemical vapour deposition technique (CVD) is the important method for preparing high-quality graphene film
One of, with the development of technology of preparing, the yield of CVD method can also meet the requirement of large-scale production.CVD can be utilized
Gaseous state, liquid, solid matter carry out the growth of graphene film as carbon source.But its method is cumbersome, high cost.Oxidation-reduction method
Including graphite oxidation is obtained into graphite oxide, then the graphene nanometer sheet for preparing different size is reduced by reducing process.So
And the limitation due to oxide-reduction method in itself, the Graphene quality prepared is relatively low (such as electrical conductivity only ＞ 1500S/m),
Graphene defect is more, has a strong impact on the performance of its performance.
At present, the preparation method of three-dimensional grapheme of the prior art is all preferable not to the utmost, is utilized the invention provides one kind
The preparation method of the three-dimensional grapheme film that single-layer graphene is constructed, obtained film has high-specific surface area, can be with metal oxygen
As electrode materials such as ultracapacitor, lithium ion battery, thin-film solar cells after compound, metal sulfide modification.
The content of the invention
In view of the shortcomings of the prior art, the present invention proposes the three-dimensional grapheme that a kind of utilization single-layer graphene is constructed
The preparation method and application of film.It is characterized in that：Ultrasound is added in the improvement Hummer method technical process for prepare Graphene
Crush and ball milling stripping technology, obtain the Graphene of individual layer or few layer, Graphene slurry is mixed with out with organic solvent, with silk
The method of wire mark brush prints the Graphene slurry of different-thickness in substrate, and this substrate for being printed with Graphene slurry is placed in
Muffle furnace, with obtained after the method for high-temperature heat treatment removal organic ink a kind of interconnection, with nano level porous three-dimensional knot
The graphene film of structure.The film has high-specific surface area, as super electricity after being modified using metal oxide, metal sulfide
The electrode materials such as container, lithium ion battery, thin-film solar cells.
The technical scheme is that：
A kind of preparation method of the three-dimensional grapheme film that utilization single-layer graphene is constructed, comprises the following steps：
(1) Hummer methods are improved and prepares redox Graphene
Low-temp reaction：Measure the concentrated sulfuric acid and pour into conical flask, be put into ice-water bath and be cooled to, native graphite and sodium nitrate are poured into
Conical flask, ultrasound a period of time, is slowly added to potassium permanganate 3g, is being stirred 2 hours less than 10 DEG C.
Middle temperature reaction：Conical flask moves to 38 DEG C of water-baths, stirring reaction 2 hours.
Pyroreaction：Resulting solution is added 100ml low temperature deionized waters, 80 DEG C of water-baths 0.5 hour are subsequently adding 60ml
Deionized water terminating reaction；The hydrogenperoxide steam generator that 25ml volume ratios are 30% is subsequently added, 40ml volume ratios are added after 15min
It is 10% hydrochloric acid solution.Centrifugation 1000 turns/min washing removal acid ions, are detected without white precipitate with barium chloride.
The reduction of graphene oxide：45 DEG C of drying of drying box obtain sheet sample, are milled into powder and are put into crucible.By crucible
It is put into the Muffle furnace 2min that temperature DEG C is for 300 DEG C.Obtain fluffy graphene powder.
Ball-milling treatment：1) dry fluffy graphene powder 0.02g is accurately weighed, organic solvent or pure water is added to
In, after stirring in ultrasonic cleaner ultrasonic disperse 10min, make graphene powder dispersed in a solvent.2) will be uniform
Dispersion graphene powder suspension in a solvent is together fitted into ball grinder together with zirconium oxide balls, is placed in planetary ball mill
Inside carry out ball milling.Control rotating speed strengthens shearing force to reduce abrading-ball shock ratio in the normal direction.Finally by after ball milling
After graphene dispersing solution suction filtration is dried, single-layer graphene powder is obtained.
(2) preparation of three-dimensional grapheme film
The preparation of Graphene slurry：It is the ethanol solution of the ethyl cellulose of 5%-15% to prepare mass fraction, and stirring is equal
9.6g terpinols and 9.2g absolute ethyl alcohols are added after even.It is eventually adding the mono-layer graphite after ready 0.05-0.1g ball millings
Alkene powder.Magnetic agitation 20-30min, then ultrasonic disperse 20min, alternately 3-5 times.Then it is stirred for evaporating dry absolute ethyl alcohol.Again
Graphene slurry is obtained after adding 0.6ml acetylacetone,2,4-pentanediones and 0.6ml OP emulsifier for mixing uniform.
Silk-screen printing prints multi-layer graphene slurry to electrode method in the FTO glass conducting surface for cleaning up, and places drum
80-120 DEG C of pretreatment 20min of wind drying box.Then printing is repeated.Last 100-150 DEG C DEG C of curing process.It is different in printing
The Graphene slurry of the number of plies.It is last in Muffle furnace 100-400 DEG C be not heat-treated at equality of temperature DEG C.
The described low-temp reaction stage introduces Ultrasonic Pulverization technology, and conical flask is poured into the 23ml concentrated sulfuric acids are measured, and is put into ice
Water-bath is cooled to 4-0 DEG C, and 1g native graphites and 0.5g sodium nitrate are poured into conical flask, opens ultrasound, and ultrasound is closed after 0.5-2h.
Finally prepare redox graphene powder.
Redox graphene powder is peeled off using ball milling, the ball material of cobalt oxide ball milling pearl and redox graphene powder
Mass ratio is about 2000:1 to 10000:1, rotating speed is 200-400 revs/min, Ball-milling Time 10-30h.
Prepared as organic solvent using including but is not limited to OP emulsifying agents, terpinol, acetylacetone,2,4-pentanedione and ethyl cellulose
Graphene slurry；
The conductive substrates for being printed with Graphene slurry are placed in warm DEG C of air dry oven pretreatment for 80-120 DEG C；
The conductive substrates for being printed with Graphene slurry are placed in Muffle furnace, and the temperature DEG C of heat treatment is 100-400 DEG C；
The three-dimensional grapheme film that the present invention is obtained has porous three-dimensional interconnection architecture, with high-specific surface area, height
Transmitance and low-resistivity.This graphene film can be directly ultracapacitor, lithium ion battery, thin-film solar cells
With the electrode material such as DSSC.
The graphene film modified with some metal oxides or metal sulfide can as ultracapacitor, lithium-ion electric
Pond is thin, the electrode material of film solar cell and DSSC etc..
Brief description of the drawings
Fig. 1 is single-layer graphene TEM photos
Fig. 2 is single-layer graphene thickness chart
Fig. 3 schemes for three-dimensional grapheme film sections SEM
Fig. 4 schemes for three-dimensional grapheme film surface SEM
Specific embodiment
(1) Hummer methods are improved and prepares redox Graphene
Low-temp reaction：Measure the 23ml concentrated sulfuric acids and pour into conical flask, be put into ice-water bath and be cooled to less than 4 DEG C, 1g natural stones
Ink and 0.5g sodium nitrate pour into conical flask, open ultrasound, and ultrasound is closed after one hour, are slowly added to potassium permanganate 3g, are being less than
10 DEG C are stirred 2 hours.
Middle temperature reaction：Conical flask moves to 38 DEG C of water-baths, stirring reaction 2 hours.
Pyroreaction：Resulting solution is added 100ml low temperature deionized waters, 80 DEG C of water-baths 0.5 hour are subsequently adding 60ml
Deionized water terminating reaction；The hydrogenperoxide steam generator that 25ml volume ratios are 30% is subsequently added, 40ml volume ratios are added after 15min
It is 10% hydrochloric acid solution.Centrifugation 1000 turns/min washing removal acid ions, are detected without white precipitate with barium chloride.
The reduction of graphene oxide：45 DEG C of drying of drying box obtain sheet sample, are milled into powder and are put into crucible.By crucible
It is put into the Muffle furnace 2min that temperature DEG C is for 300 DEG C.Obtain fluffy graphene powder.
Ball-milling treatment：1) dry graphene powder 0.02g is accurately weighed, is added in 80ml alcohol solvents or pure water,
After stirring in ultrasonic cleaner ultrasonic disperse 10min, make graphene powder dispersed in organic solvent.2) will be uniform
Dispersion graphene microchip suspension in organic solvent is together fitted into ball grinder that (ball material mass ratio is about together with zirconium oxide balls
It is 20000:1), being placed in carries out ball milling in planetary ball mill.Rotating speed is controlled at 300 revs/min to reduce abrading-ball in normal side
Upward shock ratio, strengthens shearing force；Ball-milling Time 30h.After finally the graphene dispersing solution suction filtration after ball milling is dried, obtain
To single-layer graphene powder.
(2) preparation of three-dimensional grapheme film
The preparation of Graphene slurry：Configuration quality fraction is the ethanol solution of the ethyl cellulose of 5%-15%, and stirring is equal
9.6g terpinols and 9.2g absolute ethyl alcohols are added after even.It is eventually adding ready 0.05-0.1g single-layer graphenes powder.Magnetic
Power stirs 20-30min, then ultrasonic disperse 20min, alternately 3-5 times.Then it is stirred for evaporating dry absolute ethyl alcohol.Add 0.6ml
Graphene slurry is obtained after acetylacetone,2,4-pentanedione and 0.6ml OP emulsifier for mixing are uniform.
Silk-screen printing prints multi-layer graphene slurry to electrode method in the FTO glass conducting surface for cleaning up, and places drum
80-120 DEG C of pretreatment 20min of wind drying box.Then printing is repeated.Last 100-150 DEG C DEG C of curing process.It is different in printing
The Graphene slurry of the number of plies.It is last in Muffle furnace 100-400 DEG C be not heat-treated at equality of temperature DEG C
Specific embodiment of the invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can within the scope of the claims make various deformations or amendments, this not shadow
Sound substance of the invention.
Claims (9)
1. a kind of preparation method of the three-dimensional grapheme film that utilization single-layer graphene is constructed, comprises the following steps：
(1) Hummer methods are improved and prepares redox Graphene
Native graphite and sodium nitrate obtain graphene oxide by low-temp reaction, the reaction of middle temperature, pyroreaction；
The reduction of graphene oxide：45 DEG C of drying of drying box obtain sheet sample, are milled into powder and are put into crucible.Crucible is put into
Temperature is 300 DEG C of Muffle furnace 2min.Obtain fluffy graphene powder；
Ball-milling treatment：1) dry graphene powder 0.02g is accurately weighed, is added in ethanol or pure water, in ultrasound after stirring
Ultrasonic disperse 10min in ripple washer, makes graphene powder dispersed in a solvent；2) by dispersed stone in a solvent
Black alkene powder suspension is together fitted into ball grinder together with zirconium oxide balls, and being placed in carries out ball milling in planetary ball mill；Control
Rotating speed strengthens shearing force to reduce abrading-ball shock ratio in the normal direction；Finally the graphene dispersing solution after ball milling is taken out
Be filtered dry it is dry after, obtain single-layer graphene powder.
(2) preparation of three-dimensional grapheme film
The preparation of Graphene slurry：It is the ethanol solution of the ethyl cellulose of 5%-15% to prepare mass fraction, after stirring
Add 9.6g terpinols and 9.2g absolute ethyl alcohols；It is eventually adding ready 0.05-0.1g single-layer graphenes powder；Magnetic force is stirred
20-30min, then ultrasonic disperse 20min are mixed, alternately 3-5 times；Then it is stirred for evaporating dry absolute ethyl alcohol；Add 0.6ml acetyl
Graphene slurry is obtained after acetone and 0.6ml OP emulsifier for mixing are uniform；
Silk-screen printing prints multi-layer graphene slurry to electrode method in the FTO glass conducting surface for cleaning up, and places air blast and does
Dry case pre-processes 20min；Then printing is repeated；Last 100-150 DEG C of curing process；The Graphene slurry of the different numbers of plies in printing
Material；Finally it is heat-treated in Muffle furnace.
2. the preparation method of the three-dimensional grapheme film that a kind of utilization single-layer graphene according to claim 1 is constructed, its
It is characterised by, described low-temp reaction：Conical flask is poured into the 23ml concentrated sulfuric acids are measured, ice-water bath is put into and is cooled to 4-0 DEG C, 1g
Native graphite and 0.5g sodium nitrate pour into conical flask, open ultrasound, and ultrasound is closed after 0.5-2h；Potassium permanganate 3g is slowly added to,
Stirred 2 hours less than 10 DEG C；
Middle temperature reaction：Conical flask moves to 38 DEG C of water-baths, stirring reaction 2 hours；
Pyroreaction：Resulting solution is added 100ml low temperature deionized waters, 80 DEG C of water-baths 0.5 hour, be subsequently adding 60ml go from
Sub- water terminating reaction；The hydrogenperoxide steam generator that 25ml volume ratios are 30% is subsequently added, addition 40ml volume ratios are after 15min
10% hydrochloric acid solution；Centrifugation 1000 turns/min washing removal acid ions, are detected without white precipitate with barium chloride.
3. the preparation method of the three-dimensional grapheme film that a kind of utilization single-layer graphene according to claim 1 is constructed, its
It is characterised by, it is characterised in that：Redox graphene powder is using ball milling stripping, cobalt oxide ball milling pearl and redox graphite
The ball material mass ratio of alkene powder is about 2000:1 to 10000:1, rotating speed is 200-400 revs/min, Ball-milling Time 10-30h.
4. the preparation method of the three-dimensional grapheme film that a kind of utilization single-layer graphene according to claim 1 is constructed, its
It is characterised by, is prepared as organic solvent using including but is not limited to OP emulsifying agents, terpinol, acetylacetone,2,4-pentanedione and ethyl cellulose
Graphene slurry.
5. the preparation method of the three-dimensional grapheme film that a kind of utilization single-layer graphene according to claim 1 is constructed, its
It is characterised by, the conductive substrates for being printed with Graphene slurry are placed in air dry oven pretreatment temperature for 80-120 DEG C.
6. the preparation method of the three-dimensional grapheme film that a kind of utilization single-layer graphene according to claim 1 is constructed, its
It is characterised by, the conductive substrates for being printed with Graphene slurry are placed in Muffle furnace, and the temperature of heat treatment is 100-400 DEG C.
7. the three-dimensional grapheme film that the preparation method according to claim any one of 1-6 is prepared.
8. the application of the three-dimensional grapheme film that a kind of utilization single-layer graphene according to claim 7 is constructed, its feature
Be, this graphene film can be directly ultracapacitor, lithium ion battery, thin-film solar cells and dye sensitization too
The electrode material of positive energy battery.
9. the application of the three-dimensional grapheme film that a kind of utilization single-layer graphene according to claim 7 is constructed, its feature
Be, the graphene film modified with some metal oxides or metal sulfide can as ultracapacitor, lithium ion battery
The electrode material of thin, film solar cell and DSSC.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107539984A (en) * | 2017-10-19 | 2018-01-05 | 苏州方卓材料科技有限公司 | The preparation method of graphite material |
| CN107833759A (en) * | 2017-10-13 | 2018-03-23 | 南京旭羽睿材料科技有限公司 | A kind of silk screen print method prepares the preparation method of graphene electrode of super capacitor |
| CN109671846A (en) * | 2018-11-23 | 2019-04-23 | 上海工程技术大学 | Perovskite solar battery and its preparation using three-dimensional structure graphene as back electrode |
| WO2019103409A1 (en) * | 2017-11-21 | 2019-05-31 | 주식회사 엘지화학 | Method for manufacture of sulfur-carbon composite |
| CN110739155A (en) * | 2019-09-24 | 2020-01-31 | 广东工业大学 | nickel sulfide/graphene composite film and preparation method and application thereof |
| CN112945997A (en) * | 2021-02-01 | 2021-06-11 | 天津艾克凯胜石墨烯科技有限公司 | Sample preparation method for aqueous graphene slurry before scanning electron microscope |
| CN113068280A (en) * | 2020-01-02 | 2021-07-02 | 中国科学院福建物质结构研究所 | Graphene heating film and preparation method and application thereof |
| CN115616016A (en) * | 2022-12-14 | 2023-01-17 | 矿冶科技集团有限公司 | Electronic probe sample surface conductivity treatment method |
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| CN107833759A (en) * | 2017-10-13 | 2018-03-23 | 南京旭羽睿材料科技有限公司 | A kind of silk screen print method prepares the preparation method of graphene electrode of super capacitor |
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| CN109671846A (en) * | 2018-11-23 | 2019-04-23 | 上海工程技术大学 | Perovskite solar battery and its preparation using three-dimensional structure graphene as back electrode |
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| CN110739155A (en) * | 2019-09-24 | 2020-01-31 | 广东工业大学 | nickel sulfide/graphene composite film and preparation method and application thereof |
| CN110739155B (en) * | 2019-09-24 | 2021-10-19 | 广东工业大学 | Nickel sulfide/graphene composite film and preparation method and application thereof |
| CN113068280A (en) * | 2020-01-02 | 2021-07-02 | 中国科学院福建物质结构研究所 | Graphene heating film and preparation method and application thereof |
| CN113068280B (en) * | 2020-01-02 | 2023-03-24 | 中国科学院福建物质结构研究所 | Graphene heating film and preparation method and application thereof |
| CN112945997A (en) * | 2021-02-01 | 2021-06-11 | 天津艾克凯胜石墨烯科技有限公司 | Sample preparation method for aqueous graphene slurry before scanning electron microscope |
| CN115616016A (en) * | 2022-12-14 | 2023-01-17 | 矿冶科技集团有限公司 | Electronic probe sample surface conductivity treatment method |
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