CN103500661A - Preparation method and application for carbon nanotube counter electrode thin film material modified by nitrogen-doped graphene quantum dots and graphene oxide - Google Patents
Preparation method and application for carbon nanotube counter electrode thin film material modified by nitrogen-doped graphene quantum dots and graphene oxide Download PDFInfo
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- CN103500661A CN103500661A CN201310434917.8A CN201310434917A CN103500661A CN 103500661 A CN103500661 A CN 103500661A CN 201310434917 A CN201310434917 A CN 201310434917A CN 103500661 A CN103500661 A CN 103500661A
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- Y02E10/00—Energy generation through renewable energy sources
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- Y02E10/542—Dye sensitized solar cells
Abstract
The invention belongs to the technical field of energy nanometer new functional materials, and particularly relates to a preparation method and application for a carbon nanotube counter electrode thin film material modified by nitrogen-doped graphene quantum dots and graphene oxide. The preparation method includes the steps of scattering a carbon nanotube into an aqueous solution, using the graphene oxide as a surface active agent, and adding the graphene oxide into the carbon nanotube solution to form stable and even carbon nanotube scattered solution; adding the nitrogen-doped graphene quantum dots prepared in an invisible light-Fenton method into the carbon nanotube scattered solution and enabling the solution to be evenly scattered; preparing the obtained solution into a film by using a suction filtration method, carrying out high-temperature thermal treatment on the thin film to obtain a carbon nanotube thin film with a certain strength, and using the carbon nanotube thin film as the counter electrode material of a dye-sensitized solar cell. The result shows that the thin film has high photoelectric converting efficiency, and can become an effective electrode material for replacing precious metal Pt.
Description
Technical field
The invention belongs to the new technical field of function materials of energy nanometer, be specifically related to the preparation method of a kind of New Type of Carbon nano-tube film solar cell to electrode, adopt the standby nitrating graphene quantum dot of light-Fenton legal system, using it as active catalyst, add in carbon nano-tube film, using this film as in electrode material application DSSC, significantly improve its electricity conversion.
Background technology
Along with socioeconomic growing, energy problem becomes the matter of utmost importance of restriction development of all countries economy, solar energy is as a kind of inexhaustible, nexhaustible clean energy resource has been subject to the extensive concern of various countries' researchers, along with the development with rapid changepl. never-ending changes and improvements of nanometer technology, become the powerful motive force of current new type solar energy technical development.Since French scientist Becquere in 1839 finds photovoltaic effect, the history of more than 100 year has been experienced in Optical Electro-Chemistry research.The researcher of Bell Laboratory in 1954 introduces monocrystalline silicon to PN junction, has found photoelectricity, and has started thus the research field of silicon solar cell.To 20 century 70s, for the electricity conversion of the silicon solar cell of space industry, surpassed 25%.After silicon solar cell, scientist has successively been developed again various novel solar cells, these solar cells be take thin-film solar cells as main flow, comprise silicon thin film type (amorphous silicon, monocrystalline silicon, polysilicon membrane), compound semiconductor film type (GaAs, InP, CdS, CdTe, CuInGaSn), organic film type etc.Up-to-date authoritative statistics shows, the electricity conversion of monocrystaline silicon solar cell has reached 24.7%, and polysilicon is 19.8%, and amorphous silicon is that 10.1%, CdTe is 16.5 %, and CIGS is 18.4%.
Yet at present there is highly energy-consuming in the smelting of silicon, the problem of high pollution, as produce polysilicon byproduct---silicon tetrachloride is highly toxic substance.To become barren land for the soil of toppling over or bury silicon tetrachloride, have potential very big danger, not only poisonous, contaminated environment also, cost recovery is huge.Except above business-like solar cell, scientists still is being devoted to study new solar cell material and structure at present.Wherein dye sensitization solar battery (Dye-Sensitized Solar Cells is called for short DSSC) development in recent years is rapid.Its research history can be traced back to the sixties in 20th century, and German Tributsch has found that Dye Adsorption can generation current on semiconductor under certain condition.But until before 1991, the photoelectric conversion efficiency of most of dye sensitizations lower (<1%).1991, the Gratzel professor of the engineering institutes such as Lausanne, SUI height and the nanoporous TiO that his research group adopts high-specific surface area
2film is made semi-conducting electrode, makes dyestuff with organic compounds such as transition metal Ru, and selects suitable redox electrolytes matter to develop a kind of nanocrystalline DSSC, has broken through electricity conversion 7% at one stroke.Within 1993, the people such as Gratzel have reported that electricity conversion reaches 10% dye-sensitized nano solar cell again.Than silica-based solar cell, the cost that the DSSC battery is cheap with it, simple technique and relatively high photoelectric conversion efficiency and caused global extensive concern, and started research boom rapidly.
At present, in DSSC, main application has high-efficiency catalytic activity and relatively low superpotential Pt as to electrode material, but its expensive high commercial application to DSSC of preparation cost that causes is brought certain obstacle, Pt is used for a long time in acidic electrolysis bath simultaneously, also can produce the galvano-cautery phenomenon, affect stability and the useful life of DSSC.Carbon nanomaterial (carbon nano-tube, Graphene, fullerene etc.) is with high conductivity, to I at present
2corrosion resistance and to I
3-the high reaction activity of reduction becomes the most attractive substitution material, relative low price, and being expected to substitute noble metal platinum becomes the new material of DSSC to electrode.
Summary of the invention
The object of the invention is to be based on having the preparation method of high-activity carbon nano-tube film to electrode material.
The present invention adopts the nitrating graphene quantum dot to be modified carbon nano-tube first, utilize the interpolation of nitrating graphene quantum dot can significantly increase the catalytic performance of carbon nano-tube film, avoided in traditional preparation technology improving by oxidizing process the difficult problem that electric property that the method for carbon nano-tube defect causes descends, interpolation by the nitrating graphene quantum dot effectively realizes in the immovable situation of Electrical performance, the purpose that catalytic performance improves, the abundant characteristic of having brought into play carbon nano-tube high conductivity and high catalytic activity.
based on above-mentioned mechanism, first technical scheme disclosed by the invention can be summarized as:
The preparation method of a kind of efficient carbon nano-tube film solar cell to electrode material, it is characterized in that, add the graphite oxide aqueous solution as surfactant in carbon nano-tube aqueous solutions, both form even mixed liquor, the nitrating graphene quantum dot is added in described homogeneous mixture solotion, by mixed liquor suction filtration film forming, film is annealed to reduce to process can obtain the present invention's carbon nano-tube film material to be prepared again.
Described carbon nano-tube, material can be selected multi-walled carbon nano-tubes, Single Walled Carbon Nanotube, Graphene, fullerenes etc., all can be used to prepare carbon nanocapsule thin film to electrode material.
Described nitrating graphene quantum dot, adopt light-Fenton legal system standby and obtain, also can select existing other method in this area to prepare.
The preparation method of above-mentioned carbon nanotube counter electrode thin-film material, concrete steps are as follows:
(1) by carbon nanotube dispersed in aqueous solvent, be mixed with the carbon nano-tube solution that concentration range is 1mg/L-200mg/L, be uniformly mixed; Simultaneously, graphene oxide is scattered in to aqueous solvent and forms the even liquid of graphene oxide.
(2) get a little above-mentioned graphite oxide aqueous solution and be added into (graphene oxide addition and carbon nano-tube mass ratio are greater than 1:9) in carbon nano-tube aqueous solutions, mixing and stirring as surfactant.
(3) a certain amount of nitrating graphene quantum dot is added in the mixed solution of the graphene oxide of step (2) and carbon nano-tube, mixing and stirring, obtain dispersion soln.
(4) by vacuum flask suction filtration film forming for above-mentioned dispersion soln, after film is dry, from filter membrane, peel off.
(5) to the film stripped down, the reduction of annealing is again processed, and obtains final carbon nano-tube film material.
In step (1), carbon nano-tube the selection of material used can be multi-walled carbon nano-tubes or Single Walled Carbon Nanotube.
In step (5), described heat treated temperature is 300 ~ 800 ℃; Programming rate is 5 ~ 10 ℃/min; Atmosphere is nitrogen or inert gas.
in order to obtain the nitrating graphene quantum dot, the present invention discloses a kind of preparation method of nitrating graphene quantum dot, be claimed second technical scheme of the present invention, implementation method is as follows:
(1) the nitrating Graphene is joined to dense H
2sO
4with dense HNO
3mixed liquor in, solid-to-liquid ratio is 1mg/L-200mg/L, excusing from death is uniformly mixed, the reaction 5-30h, obtain reacted oxidation nitrating Graphene acid solution.
(2) above-mentioned acid solution is adopted to the vacuum flask suction filtration, and extremely neutral with the deionized water cyclic washing.
(3) get neutral oxidation nitrating graphene solution and evenly mix in the silica ware the inside with iron salt solutions, under the ultra violet lamp of 1000W, by H
2o
2join the silica ware the inside and stir with certain speed, reaction continues 0.1-2h.This step is light-Fenton method.
(4) end reaction solution step (3) obtained is dialysed 12 hours in the bag filter of 3500 Da specifications, and, by ultrasonic acceleration dialysis, obtains the solution of nitrating graphene quantum dot.
In step (1), dense H used
2sO
4with dense HNO
3ratio be 3:1.
In step (3), molysite used can be: ferric trichloride, ferric sulfate, ferric nitrate etc.
the inventive method prepares gained carbon nano-tube film solar cell and electrode material be can be applicable to the preparation assembling of DSSC, is considered as the technical scheme three that the present invention needs protection.
Nitrating graphene quantum dot prepared by the present invention is used for carbon nano-tube modified thin-film material, using it as DSSC to electrode material, result shows that this film has higher electricity conversion, may become a kind of effective ways that substitute precious metals pt.
Compared with prior art, beneficial effect of the present invention is:
(1) adopt and there is the nitrating graphene quantum dot of good catalytic as additive, under the prerequisite that does not affect the carbon nano-tube film electric property, significantly improve the catalytic performance of carbon nano-tube, efficiently solve the difficult problem that the single carbon nanomaterial catalytic performance of current employing and electric property can't be taken into account simultaneously.
(2) preparation technology of the present invention is simple, condition is easily controlled, with low cost, be suitable for that serialization is extensive, batch production.
The accompanying drawing explanation
DSSC performance test I-V curve in Fig. 1 embodiment 1.
DSSC performance test I-V curve in Fig. 2 embodiment 2.
DSSC performance test I-V curve in Fig. 3 embodiment 3.
DSSC performance test I-V curve in Fig. 4 embodiment 4.
Embodiment
embodiment 1
50mg nitrating Graphene is joined to dense H
2sO
4(30mL) with dense HNO
3(10mL) in mixed liquor, reaction 30h in gentleness ultrasonic (500W, 40 kHz); The solution adding distil water is diluted to 250ml, and with the filtering with microporous membrane acid wherein of 0.22 μ m, cyclic washing 2-3 time, then adding distil water is made into 50ml oxidation nitrating graphene solution; Get 1ml oxidation nitrating graphene solution and 0.1ml 0.5mol/L FeCl
3in the silica ware the inside, mix, under the ultra violet lamp of 1000w, by 30ml 1mol/L H
2o
2speed with 1ml/min joins silica ware the inside vigorous stirring, and reaction continues 50min; The solution that photo-Fenton reaction is obtained is dialysed 12 hours in the bag filter of 3500 Da specifications, and by ultrasonic acceleration dialysis.Finally obtain the quantum dot solution of nitrating Graphene.
Take the 0.15g carbon nano-tube and put into 50ml water, frequently stir with glass bar, beaker is placed in to the ultrasonic 30min of Ultrasound Instrument.Separately take 0.08Gg graphene oxide (GO) and be dissolved in 120ml water, frequently with glass bar, stir, then flask is placed in to the ultrasonic 6h of Ultrasound Instrument.After ultrasonic completing, get 25ml GO solution in carbon pipe mixed liquor, with glass bar, stir 5-10min, beaker is placed in to the super 60s of the ultrasonic 3h(of Ultrasound Instrument, stop 5s), make carbon pipe dispersion liquid.
Get 4ml carbon pipe dispersion liquid and mix with the 3ml quantum dot solution, by vacuum flask suction filtration film forming.Film is annealed to reduce and process.Heat treated temperature is 400 ℃; Programming rate is 5 ℃/min; Atmosphere is argon gas.
Using the film after annealing as electrode fabrication is become to DSSC, carry out the associated batteries performance test, the I-V curve is as shown in Figure 1, open circuit voltage is: 0.70V, short circuit current is: 0.004A, and electricity conversion is: 7.39%, fill factor, curve factor is: 60%.
50mg nitrating Graphene is joined to dense H
2sO
4(30mL) with dense HNO
3(10mL) in mixed liquor, reaction 30h in gentleness ultrasonic (500W, 40 kHz); The solution adding distil water is diluted to 250ml, and with the filtering with microporous membrane acid wherein of 0.22 μ m, cyclic washing 2-3 time, then adding distil water is made into 50ml oxidation nitrating graphene solution; Get 1ml oxidation nitrating graphene solution and 0.1ml 0.5mol/L FeCl
3in the silica ware the inside, mix, under the ultra violet lamp of 1000w, by 30ml 1mol/L H
2o
2speed with 1ml/min joins silica ware the inside vigorous stirring, and reaction continues 50min; The solution that photo-Fenton reaction is obtained is dialysed 12 hours in the bag filter of 3500 Da specifications, and by ultrasonic acceleration dialysis.Finally obtain the quantum dot solution of nitrating Graphene.
Take the 0.15g carbon nano-tube and put into 50ml water, frequently stir with glass bar, beaker is placed in to the ultrasonic 30min of Ultrasound Instrument.Separately take 0.08Gg graphene oxide (GO) and be dissolved in 120ml water, frequently with glass bar, stir, then flask is placed in to the ultrasonic 6h of Ultrasound Instrument.After ultrasonic completing, get 25ml GO solution in carbon pipe mixed liquor, with glass bar, stir 5-10min, beaker is placed in to the super 60s of the ultrasonic 3h(of Ultrasound Instrument, stop 5s), make carbon pipe dispersion liquid.
Get 4ml carbon pipe dispersion liquid and mix with the 2.5ml quantum dot solution, by vacuum flask suction filtration film forming.Film is annealed to reduce and process.Heat treated temperature is 400 ℃; Programming rate is 5 ℃/min; Atmosphere is argon gas.
Using the film after annealing as electrode fabrication is become to DSSC, carry out the associated batteries performance test, the I-V curve is as shown in Figure 2, open circuit voltage is: 0.72V, short circuit current is: 0.004A, and electricity conversion is: 6.25%, fill factor, curve factor is: 48.3%.
embodiment 3
50mg nitrating Graphene is joined to dense H
2sO
4(30mL) with dense HNO
3(10mL) in mixed liquor, reaction 30h in gentleness ultrasonic (500W, 40 kHz); The solution adding distil water is diluted to 250ml, and with the filtering with microporous membrane acid wherein of 0.22 μ m, cyclic washing 2-3 time, then adding distil water is made into 50ml oxidation nitrating graphene solution; Get 1ml oxidation nitrating graphene solution and 0.1ml 0.5mol/L FeCl
3in the silica ware the inside, mix, under the ultra violet lamp of 1000w, by 30ml 1mol/L H
2o
2speed with 1ml/min joins silica ware the inside vigorous stirring, and reaction continues 50min; The solution that photo-Fenton reaction is obtained is dialysed 12 hours in the bag filter of 3500 Da specifications, and by ultrasonic acceleration dialysis.Finally obtain the quantum dot solution of nitrating Graphene.
Take the 0.15g carbon nano-tube and put into 50ml water, frequently stir with glass bar, beaker is placed in to the ultrasonic 30min of Ultrasound Instrument.Separately take 0.08Gg graphene oxide (GO) and be dissolved in 120ml water, frequently with glass bar, stir, then flask is placed in to the ultrasonic 6h of Ultrasound Instrument.After ultrasonic completing, get 25ml GO solution in carbon pipe mixed liquor, with glass bar, stir 5-10min, beaker is placed in to the super 60s of the ultrasonic 3h(of Ultrasound Instrument, stop 5s), make carbon pipe dispersion liquid.
Get 4ml carbon pipe dispersion liquid and mix with the 1ml quantum dot solution, by vacuum flask suction filtration film forming.Film is annealed to reduce and process.Heat treated temperature is 400 ℃; Programming rate is 5 ℃/min; Atmosphere is argon gas.
Using the film after annealing as electrode fabrication is become to DSSC, carry out the associated batteries performance test, the I-V curve is as shown in Figure 2, open circuit voltage is: 0.63V, short circuit current is: 0.004A, and electricity conversion is: 6.0%, fill factor, curve factor is: 52.9%.
embodiment 4
50mg nitrating Graphene is joined to dense H
2sO
4(30mL) with dense HNO
3(10mL) in mixed liquor, reaction 30h in gentleness ultrasonic (500W, 40 kHz); The solution adding distil water is diluted to 250ml, and with the filtering with microporous membrane acid wherein of 0.22 μ m, cyclic washing 2-3 time, then adding distil water is made into 50ml oxidation nitrating graphene solution; Get 1ml oxidation nitrating graphene solution and 0.1ml 0.5mol/L FeCl
3in the silica ware the inside, mix, under the ultra violet lamp of 1000w, by 30ml 1mol/L H
2o
2speed with 1ml/min joins silica ware the inside vigorous stirring, and reaction continues 50min; The solution that photo-Fenton reaction is obtained is dialysed 12 hours in the bag filter of 3500 Da specifications, and by ultrasonic acceleration dialysis.Finally obtain the quantum dot solution of nitrating Graphene.
Take the 0.15g carbon nano-tube and put into 50ml water, frequently stir with glass bar, beaker is placed in to the ultrasonic 30min of Ultrasound Instrument.Separately take 0.08Gg graphene oxide (GO) and be dissolved in 120ml water, frequently with glass bar, stir, then flask is placed in to the ultrasonic 6h of Ultrasound Instrument.After ultrasonic completing, get 25ml GO solution in carbon pipe mixed liquor, with glass bar, stir 5-10min, beaker is placed in to the super 60s of the ultrasonic 3h(of Ultrasound Instrument, stop 5s), make carbon pipe dispersion liquid.
Get 4ml carbon pipe dispersion liquid and mix with 0.2ml nitrating graphene solution, by vacuum flask suction filtration film forming.Film is annealed to reduce and process.Heat treated temperature is 400 ℃; Programming rate is 5 ℃/min; Atmosphere is argon gas.
Using the film after annealing as electrode fabrication is become to DSSC, carry out the associated batteries performance test, the I-V curve is as shown in Figure 2, open circuit voltage is: 0.69V, short circuit current is: 0.004A, and electricity conversion is: 6.75%, fill factor, curve factor is: 54.6%.
Claims (4)
1. the efficient carbon nano-tube film solar cell preparation method to electrode material, it is characterized in that, add the graphite oxide aqueous solution as surfactant in carbon nano-tube aqueous solutions, both form even mixed liquor, the nitrating graphene quantum dot is added in described homogeneous mixture solotion, by mixed liquor suction filtration film forming, film is annealed to reduce to process can obtain the present invention's carbon nano-tube film material to be prepared again.
2. preparation method as claimed in claim 1, is characterized in that, concrete steps are as follows:
(1) by carbon nanotube dispersed in aqueous solvent, be mixed with the carbon nano-tube solution that concentration range is 1mg/L-200mg/L, be uniformly mixed; Simultaneously, graphene oxide is scattered in to aqueous solvent and forms the even liquid of graphene oxide;
(2) get a little above-mentioned graphite oxide aqueous solution and be added in carbon nano-tube aqueous solutions as surfactant, mixing and stirring;
；
(3) a certain amount of nitrating graphene quantum dot is added in the mixed solution of the graphene oxide of step (2) and carbon nano-tube, mixing and stirring, obtain dispersion soln;
(4) by vacuum flask suction filtration film forming for above-mentioned dispersion soln, after film is dry, from filter membrane, peel off;
(5) to the film stripped down, the reduction of annealing is again processed, and obtains final carbon nano-tube film material.
3. the preparation method of a nitrating graphene quantum dot, is characterized in that, comprises that step is as follows:
(1) the nitrating Graphene is joined to dense H
2sO
4with dense HNO
3mixed liquor in, solid-to-liquid ratio is 1mg/L-200mg/L, excusing from death is uniformly mixed, the reaction 5-30h, obtain reacted oxidation nitrating Graphene acid solution;
(2) above-mentioned acid solution is adopted to the vacuum flask suction filtration, and extremely neutral with the deionized water cyclic washing;
(3) get neutral oxidation nitrating graphene solution and evenly mix in the silica ware the inside with iron salt solutions, under the ultra violet lamp of 1000W, by H
2o
2join the silica ware the inside and stir with certain speed, reaction continues 0.1-2h;
(4) end reaction solution step (3) obtained is dialysed 12 hours in the bag filter of 3500 Da specifications, and, by ultrasonic acceleration dialysis, obtains the solution of nitrating graphene quantum dot.
4. prepare gained carbon nano-tube film solar cell by claim 1 or 2 described methods and electrode material is applied to the preparation assembling of DSSC.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103903861A (en) * | 2014-04-23 | 2014-07-02 | 南开大学 | Counter electrode made of metal sulfide and graphene composite materials and preparation method and application of counter electrode |
| CN105334253A (en) * | 2015-12-03 | 2016-02-17 | 福建医科大学 | Method of testing PML/RAR alpha genes through electrochemical biosensor of carbon dot @ graphene oxide composite material |
| CN106602012A (en) * | 2016-12-13 | 2017-04-26 | 上海交通大学 | Flexible thin-film electrode and preparation method and application thereof |
| CN106653384A (en) * | 2016-08-29 | 2017-05-10 | 上海大学 | Preparation method for amino functional graphene quantum dot/carbon nanotube/carbon cloth three-dimensional flexible electrode |
| CN106810823A (en) * | 2017-01-18 | 2017-06-09 | 武汉工程大学 | Graphene quantum dot/CNT/PEDOT:PSS composite film and preparation method thereof |
| CN107043104A (en) * | 2017-05-11 | 2017-08-15 | 桂林理工大学 | A kind of graphene quantum dot induces high nitrogen doped photo-reduction graphene oxide preparation method |
| CN107068407A (en) * | 2017-01-03 | 2017-08-18 | 武汉市三选科技有限公司 | DSSC and its manufacture method |
| CN109453679A (en) * | 2018-10-30 | 2019-03-12 | 江苏理工学院 | A kind of preparation method of nitrating graphene oxide titanium dioxide composite hyperfiltration membrane |
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| CN105334253A (en) * | 2015-12-03 | 2016-02-17 | 福建医科大学 | Method of testing PML/RAR alpha genes through electrochemical biosensor of carbon dot @ graphene oxide composite material |
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| CN106602012B (en) * | 2016-12-13 | 2020-05-26 | 上海交通大学 | Flexible thin film electrode and preparation method and application thereof |
| CN107068407A (en) * | 2017-01-03 | 2017-08-18 | 武汉市三选科技有限公司 | DSSC and its manufacture method |
| CN106810823A (en) * | 2017-01-18 | 2017-06-09 | 武汉工程大学 | Graphene quantum dot/CNT/PEDOT:PSS composite film and preparation method thereof |
| CN107043104A (en) * | 2017-05-11 | 2017-08-15 | 桂林理工大学 | A kind of graphene quantum dot induces high nitrogen doped photo-reduction graphene oxide preparation method |
| CN109453679A (en) * | 2018-10-30 | 2019-03-12 | 江苏理工学院 | A kind of preparation method of nitrating graphene oxide titanium dioxide composite hyperfiltration membrane |
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Application publication date: 20140108 |