CN103172062A - Preparation method of graphene film for dye-sensitized solar cell counter electrodes - Google Patents
Preparation method of graphene film for dye-sensitized solar cell counter electrodes Download PDFInfo
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- CN103172062A CN103172062A CN2013101323585A CN201310132358A CN103172062A CN 103172062 A CN103172062 A CN 103172062A CN 2013101323585 A CN2013101323585 A CN 2013101323585A CN 201310132358 A CN201310132358 A CN 201310132358A CN 103172062 A CN103172062 A CN 103172062A
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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
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- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/542—Dye sensitized solar cells
Abstract
The invention discloses a preparation method of a graphene film for dye-sensitized solar cell counter electrodes. The method comprises the following concrete steps: firstly preparing graphite oxide aqueous solution through a Hummers method, then adding N, N-dimethyl formamide (DMF) serving as dispersing agent into the graphite oxide aqueous solution to obtain stable grapheme oxide dispersion liquid through an ultrasonic stripping method, directly depositing the graphene film on a preheated conducting substrate through a spraying method, and finally reducing the graphene film through a hydrazine steam chemical reduction method and high-temperature calcination technology, so as to obtain the graphene film for counter electrodes. The graphene film prepared through the method not only has higher electrical conductivity and can effectively transmit electron, but also has the characteristics of good uniformity, low cost and high production efficiency, and can preliminarily replace expensive platinum counter electrodes.
Description
Technical field
The present invention relates to novel material Graphene (Graphene) thin film technology technology, be specifically related to a kind of dye sensitization solar battery to the preparation method of electrode with graphene film, belong to the nanometer field of energy source materials.
Background technology
Graphene (Graphene) be by carbon atom with
sp 2The two dimensional crystal material that the monoatomic layer that hydridization connects consists of, wherein carbon atom is arranged in the Graphene plane with hexa-atomic annular preiodic type.In Graphene, the motion of electronics as the motion of theory of relativity massless particle, is followed the rule of linear diffusion simultaneously, therefore causes Graphene to have the electrology characteristic of many novelties.The electric property of Graphene is highly stable, does not vary with temperature, and is subjected to the impact of environment also very little, and electronic mobility is up to 10
4cm
2/ Vs.All the time, dye sensitization solar battery is the conductive substrates of platinum plating to electrode, although platinum has conductive capability preferably to electrode, well-known, the use cost of platinum is high.This makes in recent years, and the research to electrode begins to come into one's own extremely abundant Graphene (Graphene) material in source as dye sensitization solar battery.For example, high congruent people [the Electrochemistry Communications of Tsing-Hua University's stone in 2008,10 (2008) 1555 – 1558] utilize spin-coating method to prepare the Graphene dye sensitization solar battery to electrode conductive film, obtained excellent photoelectric transformation efficiency; Hubei University's king's generation in 2011 is quick waits people [Solid State Sciences, 13 (2011) 468 – 475] to utilize suction method to prepare the Graphene dye sensitization solar battery to electrode conductive film, has also obtained excellent photoelectric transformation efficiency.Yet spin-coating method or suction method all can not big area prepare graphene film to electrode, the pulling film forming technology that occurs subsequently can realize large-area film preparation, but being used for the graphene solution of pulling film forming reunites seriously, is difficult to obtain big area, graphene film uniformly.
Summary of the invention
The technical problem that solves:Purpose of the present invention be exactly for above-mentioned to the deficiency of electrode with the graphene film present Research, a kind of big area, the preparation method of graphene film to electrode uniformly of realizing is provided.
Technical scheme:A kind of dye sensitization solar battery is to the preparation method of electrode with graphene film, adopt N, dinethylformamide (DMF) effectively disperses the graphite oxide aqueous solution as dispersion agent, then adopt spray method directly to deposit graphene oxide film on the conductive substrates of preheating, at last by technique oxidation graphene films such as hydrazine steam chemical reduction method and high-temperature calcinations to obtain the electrode graphene film.
Concrete preparation process is: (1) at first adopts the standby graphite oxide that obtains of Hummers legal system, adopts rotating speed 10000 rpm centrifugation gained graphite oxides and uses the deionized water repetitive scrubbing, and obtaining concentration is the graphite oxide aqueous solution of 1 ~ 10 mg/mL; (2) add N in the graphite oxide aqueous solution, dinethylformamide (DMF) solution is as dispersion agent, and utilize ultrasonic stripping method to obtain the graphite oxide aqueous solution of stably dispersing, and the power of ultrasonic oscillator is 800 W, hyperacoustic frequency is 10 kHz; (3) utilizing spray method is on the conductive substrates of 150 ~ 300 ℃, to obtain graphene oxide film in preheating temperature with graphite oxide aqueous solution Direct precipitation; (4) graphene oxide film being placed in the baking oven of 25 ℃ dries; then put into hydrazine steam chemical reduction 6 ~ 15 h; and then be warming up to 400 ~ 500 ℃ in the mixed gas protected High Temperature Furnaces Heating Apparatus of hydrogen/argon gas; be down to room temperature after being incubated 1 h, obtain dye sensitization solar battery to the electrode graphene film.
The amount of adding DMF in described step (2) accounts for 0.1 ~ 1.0% of graphite oxide aqueous solution volume.
In described step (3), the spray gun bore is 0.2 ~ 0.4 mm, and the gun slot flow velocity is 2 ~ 5 mL/min, and spray time is 5 ~ 60 s.
In described step (4), the volume percent example of high temperature reduction shielding gas argon gas and hydrogen gas mixture is 5 ~ 9; intensification and rate of temperature fall are 0.5 ~ 5 ℃/min, and the gained dye sensitization solar battery is advisable at 20 ~ 300 nm with the thickness of graphene film to electrode.
Beneficial effect:Compare with existing method for preparing graphene membrane, the present invention has following characteristics: the present invention adopts graphene oxide solution rather than graphene solution as spray solution, has avoided the generation of reuniting; Secondly by DMF (DMF), graphene oxide is effectively disperseed, further prevented the generation of reuniting, avoided forming inhomogeneous nano structure membrane to electrode in the sprayed deposit process.
Description of drawings
Fig. 1 is the SEM photo to electrode use graphene film that adopts spray deposition to obtain;
Fig. 2 shows be to electrode be the dye sensitization solar battery that assembles of graphene film current density-voltage (
I-V) test curve.Wherein X-coordinate is voltage, and unit is volt (V), and ordinate zou is current density, and unit is mA/cm
2
Embodiment
The invention will be further described below in conjunction with example, but the present invention is not limited to following examples.
Embodiment 1:
(1) at first adopt the standby graphite oxide that obtains of Hummers legal system, centrifugation gained graphite oxide is also used the deionized water repetitive scrubbing, and obtaining concentration is the graphite oxide aqueous solution of 1 mg/mL;
(2) adding volumn concentration in the graphite oxide aqueous solution is 0.1% N, dinethylformamide (DMF) solution is as dispersion agent, and utilize ultrasonic stripping method to obtain the graphite oxide aqueous solution of stably dispersing, the power of ultrasonic oscillator is 800 W, and hyperacoustic frequency is 10 kHz;
(3) regulating the spray gun bore is 0.2 mm, and flow velocity is 2 mL/min, and utilizing spray method is that in the ITO conductive glass substrate of 150 ℃, spray time is 5 s, obtains graphene oxide film in preheating temperature with graphite oxide aqueous solution Direct precipitation;
(4) graphene oxide film being placed in the baking oven of 25 ℃ dries; then put into hydrazine steam chemical reduction 6 h; and then be slowly to be warming up to 400 ℃ in the mixed gas protected High Temperature Furnaces Heating Apparatus of hydrogen/argon gas of 5 in volume percent; slowly be down to room temperature after being incubated 1 h, obtain thickness and be the dye sensitization solar battery of 20 nm to the electrode graphene film.
?
Embodiment 2:
(1) at first adopt the standby graphite oxide that obtains of Hummers legal system, centrifugation gained graphite oxide is also used the deionized water repetitive scrubbing, and obtaining concentration is the graphite oxide aqueous solution of 3 mg/mL;
(2) adding volumn concentration in the graphite oxide aqueous solution is 0.5% N, dinethylformamide (DMF) solution is as dispersion agent, and utilize ultrasonic stripping method to obtain the graphite oxide aqueous solution of stably dispersing, the power of ultrasonic oscillator is 800 W, and hyperacoustic frequency is 10 kHz;
(3) regulating the spray gun bore is 0.3 mm, and flow velocity is 3 mL/min, and utilizing spray method is that in the ITO conductive glass substrate of 200 ℃, spray time is 20 s, obtains graphene oxide film in preheating temperature with graphite oxide aqueous solution Direct precipitation;
(4) graphene oxide film being placed in the baking oven of 25 ℃ dries; then put into hydrazine steam chemical reduction 6 h; and then be slowly to be warming up to 450 ℃ in the mixed gas protected High Temperature Furnaces Heating Apparatus of hydrogen/argon gas of 6 in volume percent; slowly be down to room temperature after being incubated 1 h, obtain thickness and be the dye sensitization solar battery of 100 nm to the electrode graphene film.
?
Embodiment 3:
(1) at first adopt the standby graphite oxide that obtains of Hummers legal system, centrifugation gained graphite oxide is also used the deionized water repetitive scrubbing, obtaining concentration is the graphite oxide aqueous solution of 5 mg/mL, and the power of ultrasonic oscillator is 800 W, and hyperacoustic frequency is 10 kHz;
(2) add in the graphite oxide aqueous solution volumn concentration be 0.5% DMF (DMF) solution as dispersion agent, and utilize ultrasonic stripping method to obtain stably dispersing and the less graphite oxide aqueous solution of the number of plies;
(3) regulating the spray gun bore is 0.4 mm, and flow velocity is 3 mL/min, and utilizing spray method is that in the ITO conductive glass substrate of 300 ℃, spray time is 30 s, obtains graphene oxide film in preheating temperature with graphite oxide aqueous solution Direct precipitation;
(4) graphene oxide film being placed in the baking oven of 25 ℃ dries; then put into hydrazine steam chemical reduction 12 h; and then be slowly to be warming up to 500 ℃ in the mixed gas protected High Temperature Furnaces Heating Apparatus of hydrogen/argon gas of 9 in volume percent; slowly be down to room temperature after being incubated 1 h, obtain thickness and be the dye sensitization solar battery of 150 nm to the electrode graphene film.Scanning electronic microscope (SEM) photo of the graphene film that makes for embodiment 3 that Fig. 1 shows to electrode.
?
Embodiment 4:
(1) at first adopt the standby graphite oxide that obtains of Hummers legal system, centrifugation gained graphite oxide is also used the deionized water repetitive scrubbing, obtaining concentration is the graphite oxide aqueous solution of 10 mg/mL, and the power of ultrasonic oscillator is 800 W, and hyperacoustic frequency is 10 kHz;
(2) add in the graphite oxide aqueous solution volumn concentration be 1.0% DMF (DMF) solution as dispersion agent, and utilize ultrasonic stripping method to obtain stably dispersing and the less graphite oxide aqueous solution of the number of plies;
(3) regulating the spray gun bore is 0.4 mm, and flow velocity is 5 mL/min, and utilizing spray method is that in the ITO conductive glass substrate of 300 ℃, spray time is 60 s, obtains graphene oxide film in preheating temperature with graphite oxide aqueous solution Direct precipitation;
(4) graphene oxide film being placed in the baking oven of 25 ℃ dries; then put into hydrazine steam chemical reduction 15 h; and then be slowly to be warming up to 500 ℃ in the mixed gas protected High Temperature Furnaces Heating Apparatus of hydrogen/argon gas of 9 in volume percent; slowly be down to room temperature after being incubated 1 h, obtain thickness and be the dye sensitization solar battery of 300 nm to the electrode graphene film.
Embodiment 5:
Sprayed deposit Graphene of the present invention becomes dye sensitization solar battery to electrode assembling and carries out the experiment of photoelectric transformation efficiency test: with TiO
2The film light anode is immersed in sensitization in the N719 dyestuff of 0.3 mmol/L, insulation 1 h under 60 ℃; Be that the Surlyn heat-sealing film of 60 μ m is with TiO with thickness after sensitization
2The graphene film that film light anode and embodiment 3 prepare/ITO conductive glass is packaged into sandwich sandwich structure, and the sandwich of layers perfusion contains the DHS-E23 type electrolytic solution of iodide ion; Adopt U.S. Oriel 94022A solar simulator, at 100 mW/cm
2Intensity of illumination under the photoelectric transformation efficiency of test battery.What Fig. 2 showed is the test curve of the current-voltage (I-V) of dye sensitization solar battery.Result shows, the graphene film of the present embodiment preparation to electrode can alternative metals platinum to electrode, battery can normally move and produce photoelectric current and photovoltage.The graphene film for preparing in other embodiments of the invention all can be used as electrode is used, and after being packaged into dye sensitization solar battery, can produce effective photoelectric current and photovoltage.
Claims (5)
1. a dye sensitization solar battery is to the preparation method of electrode with graphene film, it is characterized in that: adopt N, dinethylformamide (DMF) effectively disperses the graphite oxide aqueous solution as dispersion agent, then adopt spray method directly to deposit graphene oxide film on the conductive substrates of preheating, at last by technique oxidation graphene films such as hydrazine steam chemical reduction method and high-temperature calcinations to obtain the electrode graphene film.
2. a dye sensitization solar battery is to the preparation method of electrode with graphene film, it is characterized in that preparation process is: (1) at first adopts the standby graphite oxide that obtains of Hummers legal system, adopt rotating speed 10000 rpm centrifugation gained graphite oxides and use the deionized water repetitive scrubbing, obtaining concentration is the graphite oxide aqueous solution of 1 ~ 10 mg/mL; (2) add N in the graphite oxide aqueous solution, dinethylformamide (DMF) solution is as dispersion agent, and utilize ultrasonic stripping method to obtain the graphite oxide aqueous solution of stably dispersing, and the power of ultrasonic oscillator is 800 W, hyperacoustic frequency is 10 kHz; (3) utilizing spray method is on the conductive substrates of 150 ~ 300 ℃, to obtain graphene oxide film in preheating temperature with graphite oxide aqueous solution Direct precipitation; (4) graphene oxide film being placed in the baking oven of 25 ℃ dries; then put into hydrazine steam chemical reduction 6 ~ 15 h; and then be warming up to 400 ~ 500 ℃ in the mixed gas protected High Temperature Furnaces Heating Apparatus of hydrogen/argon gas; be down to room temperature after being incubated 1 h, obtain dye sensitization solar battery to the electrode graphene film.
3. a kind of dye sensitization solar battery according to claim 2 to the preparation method of electrode with graphene film, is characterized in that the amount of adding DMF in described step (2) accounts for 0.1 ~ 1.0% of graphite oxide aqueous solution volume.
4. a kind of dye sensitization solar battery according to claim 2 is to the preparation method of electrode with graphene film, it is characterized in that in described step (3), the spray gun bore is 0.2 ~ 0.4 mm, the gun slot flow velocity is 2 ~ 5 mL/min, and spray time is 5 ~ 60 s.
5. a kind of dye sensitization solar battery according to claim 2 is to the preparation method of electrode with graphene film; the volume percent example that it is characterized in that the middle high temperature reduction shielding gas argon gas of described step (4) and hydrogen gas mixture is 5 ~ 9; intensification and rate of temperature fall are 0.5 ~ 5 ℃/min, and the gained dye sensitization solar battery is advisable at 20 ~ 300 nm with the thickness of graphene film to electrode.
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| CN103466612A (en) * | 2013-10-08 | 2013-12-25 | 东南大学 | Method for preparing native grapheme by means of frequency mixing ultrasound |
| CN103985546A (en) * | 2014-05-19 | 2014-08-13 | 东南大学 | Graphene-CoS nanosheet composite counter electrode and preparation method thereof |
| CN104425135A (en) * | 2013-09-05 | 2015-03-18 | 国家纳米科学中心 | Preparation method for reduced graphene oxide counter electrode and application thereof |
| CN104591164A (en) * | 2014-12-30 | 2015-05-06 | 常州碳星科技有限公司 | Method for preparing graphene microspheres |
| CN104609409A (en) * | 2015-01-22 | 2015-05-13 | 东南大学 | Preparation method of graphene millimeter sheet |
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| CN108172405A (en) * | 2018-01-09 | 2018-06-15 | 阜阳师范学院 | The method of electrochemical reduction oxidation graphene and the quasi-solid-state dye sensitized solar cell prepared using electrochemical reduction oxidation graphene |
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Patent Citations (2)
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| CN102173414A (en) * | 2011-03-18 | 2011-09-07 | 中国地质大学（武汉） | Method for preparing graphene oxide by chemical peeling |
| CN102750998A (en) * | 2012-07-09 | 2012-10-24 | 深圳市贝特瑞纳米科技有限公司 | Transparent graphene conductive thin film and preparation method thereof |
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| CN104425135A (en) * | 2013-09-05 | 2015-03-18 | 国家纳米科学中心 | Preparation method for reduced graphene oxide counter electrode and application thereof |
| CN103466612A (en) * | 2013-10-08 | 2013-12-25 | 东南大学 | Method for preparing native grapheme by means of frequency mixing ultrasound |
| CN103985546A (en) * | 2014-05-19 | 2014-08-13 | 东南大学 | Graphene-CoS nanosheet composite counter electrode and preparation method thereof |
| CN104591164A (en) * | 2014-12-30 | 2015-05-06 | 常州碳星科技有限公司 | Method for preparing graphene microspheres |
| CN104609409A (en) * | 2015-01-22 | 2015-05-13 | 东南大学 | Preparation method of graphene millimeter sheet |
| CN106252080A (en) * | 2016-07-29 | 2016-12-21 | 太原理工大学 | A kind of carbon nanomaterial is prepared as the DSSC method to electrode |
| CN106252080B (en) * | 2016-07-29 | 2019-03-12 | 太原理工大学 | A kind of carbon nanomaterial is prepared into dye-sensitized solar cells to the method for electrode |
| CN106409935A (en) * | 2016-10-19 | 2017-02-15 | 华中科技大学 | MoO3/MoS2/LiF flexible heterojunction solar cell and preparation method thereof |
| CN106409935B (en) * | 2016-10-19 | 2017-10-24 | 华中科技大学 | A kind of MoO3/MoS2/ LiF flexibility heterojunction solar batteries and preparation method thereof |
| CN106807601A (en) * | 2017-03-13 | 2017-06-09 | 中国科学院海洋研究所 | A kind of method for preparing semiconductor powder film photoelectric electrode |
| CN107603225A (en) * | 2017-10-27 | 2018-01-19 | 成都新柯力化工科技有限公司 | The graphene anti-corrosion film and preparation method of a kind of Pasting |
| CN107603225B (en) * | 2017-10-27 | 2018-11-06 | 泉州嘉德利电子材料有限公司 | A kind of the graphene anti-corrosion film and preparation method of Pasting |
| CN108172405A (en) * | 2018-01-09 | 2018-06-15 | 阜阳师范学院 | The method of electrochemical reduction oxidation graphene and the quasi-solid-state dye sensitized solar cell prepared using electrochemical reduction oxidation graphene |
| CN108172405B (en) * | 2018-01-09 | 2019-09-03 | 阜阳师范学院 | The quasi-solid-state dye sensitized solar cell prepared using electrochemical reduction oxidation graphene |
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