CN103985546A - Graphene-CoS nanosheet composite counter electrode and preparation method thereof - Google Patents

Graphene-CoS nanosheet composite counter electrode and preparation method thereof Download PDF

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Publication number
CN103985546A
CN103985546A CN201410211259.0A CN201410211259A CN103985546A CN 103985546 A CN103985546 A CN 103985546A CN 201410211259 A CN201410211259 A CN 201410211259A CN 103985546 A CN103985546 A CN 103985546A
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graphene
cos
counter electrode
graphene oxide
electrode
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徐峰
朱重阳
王豪
闵辉华
董辉
孙立涛
翟旺旺
孙博闻
谭爽
刘欣博
李潇
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Southeast University
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Southeast University
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Abstract

The invention discloses a graphene-CoS nanosheet composite counter electrode and a preparation method thereof. The graphene-CoS nanosheet composite counter electrode is composed of a graphene thin film and a CoS nanosheet array. The graphene thin film is obtained by the fact that an oxidized graphene thin film is deposited on an ITO conductive glass substrate through a spraying technology, and then electrochemical reduction is conducted. The CoS nanosheet array is directly deposited and grown on the surface of the oxidized graphene thin film in an electrochemical mode. The graphene-CoS nanosheet composite counter electrode is simple in preparation method, and has the advantages of low temperature operation, quick and large-area preparation and environment friendliness. Meanwhile, the prepared composite counter electrode has the advantages of being high in electron mobility, small in interfacial charge transfer resistance and high in catalytic activity, and the photoelectric conversion efficiency of a dye-sensitized solar cell is effectively improved.

Description

A kind of Graphene-CoS nanometer sheet combined counter electrode and preparation method thereof
Technical field
The present invention relates to a kind of used by dye sensitization solar battery Graphene-CoS nanometer sheet combined counter electrode and preparation method thereof, belong to Graphene-CoS nano compound film technology.
Background technology
Conventional dyes sensitization solar battery is mainly made up of electrode nanostructure light anode, ion electrolyte and the Pt of dye sensitization.Wherein, to the effect of electrode be from external circuit transmission electronic to redox couple I3-to I-, and to I3-to I-reduction process play important catalytic action.But, because Pt material is noble metal, and Pt content is less on earth, thereby it is significant that exploitation has the functional material of similar Pt electrochemical properties.Wherein, transient metal sulfide CoS is with its abundant microstructure, as nano particle, monodimension nano stick, two-dimensional nano sheet etc. have obtained broad research as DSSC to electrode material.But because the single nanostructure form of this class makes electrode catalyst performance and interface electric transmission be difficult to be improved simultaneously, cause the photoelectric conversion efficiency of battery limited.Thereby the research based on CoS nanostructure combined counter electrode has obtained attention.
In recent years, Graphene with the specific area of its superior electric property and super large become in DSSC, have potentiality to electrode material, the laminated film based on CoS and Graphene becomes desirable efficiently to electrode material.Document Carbon, 61 (2013) 116~123 and Carbon, 50 (2012) 485~4821 Graphenes that all proposed to prepare taking CVD are substrate, obtain the combined counter electrode of Graphene and CoS nano particle through chemical bath deposition, thereby have strengthened electronics transport capacity; Document Materials Letters, 114 (2014) 7~10 by electrophoretic deposition graphene oxide layer, more also obtains the composite construction of Graphene and CoS nano particle through chemical bath deposition.But prepare the method for laminated film and the photoelectric conversion efficiency of the combined counter electrode of gained Graphene and CoS nano particle in battery is lower based on above-mentioned.This is because at present the method for prepared Graphene-CoS combined counter electrode is mostly by chemical bath deposition CoS nano particle, the composite construction that this method is difficult to obtain that pattern is abundant, electricity and catalysis characteristics have concurrently.And other methods of preparing Graphene-CoS combined counter electrode are mainly by the operation skill in using a kitchen knife in cookery and silk screen print method, must relate to the use of the additives such as organic solvent, need to introduce high-temperature post-treatment technique and remove additive, will certainly bring adverse effect to Thin Films and performance, also have environment and potential safety hazard.For this reason, exploitation one can low-temperature operation, rapid large-area preparation, eco-friendly synthetic method, and Graphene-CoS combined counter electrode that preparation has swift electron transmission channel and high catalytic activity just has important practical value and significance.
Summary of the invention
Goal of the invention: in order to overcome the deficiencies in the prior art, the invention provides a kind of Graphene-CoS nanometer sheet of a kind of used by dye sensitization solar battery combined counter electrode and preparation method thereof, this combined counter electrode has swift electron linear transmission passage and high catalytic activity.
Technical scheme: for achieving the above object, the technical solution used in the present invention is:
A kind of used by dye sensitization solar battery Graphene-CoS nanometer sheet combined counter electrode, is made up of graphene film and CoS nano-chip arrays; Described graphene film is in the substrate of ITO electro-conductive glass, to deposit graphene oxide film by spraying coating process, then through electrochemical reduction gained; Described CoS nano-chip arrays Direct Electrochemistry deposition growing is on graphene oxide film surface.
Above-mentioned combined counter electrode, graphene film both provided large area swift electron transport layer, had increased again the catalytic reaction activity site of composite material; Quick straight line electron channel when CoS nano-chip arrays had both kept single structure, the while shows again the electrochemical catalysis enhancement effect of lower interface charge transfer resistance and Geng Gao; There is the characteristic that electron mobility is fast, interface charge transfer resistance is little, catalytic activity is high, effectively promoted the photoelectric conversion efficiency of DSSC.
Preferably, the thickness of described CoS nano-chip arrays is 0.1~2.0 μ m.
A kind of used by dye sensitization solar battery Graphene-CoS nanometer sheet combined counter electrode preparation method, first utilize Hummer's legal system for graphene oxide, ultrasonic again it is dispersed in alcohol solvent, in the substrate of ITO electro-conductive glass, deposits graphene oxide film by spraying coating process; Then taking cobalt chloride/cobaltous sulfate and thiocarbamide/thioacetamide mixed aqueous solution as electrolyte, the three electrode electro-deposition systems of the employing CoS nano-chip arrays of directly growing on graphene oxide film makes graphene oxide electrochemical reduction become Graphene simultaneously.
Said method specifically comprises the steps:
(1) utilize Hummer's legal system for graphene oxide, the graphene oxide ethanolic solution that compound concentration is 10~50mg/L deposits graphene oxide film by spraying coating process in the substrate of ITO electro-conductive glass;
(2) thiocarbamide/thioacetamide mixed aqueous solution that cobalt chloride/cobaltous sulfate that compound concentration is 5~15mM and concentration are 15~150mM is electrolyte, and gained solution is designated as A solution;
(3), taking A solution as electrolyte, adopt three electrode electro-deposition systems potentiostatic electrodeposition CoS nano-chip arrays on graphene oxide film; Electrolyte temperature is 25~55 DEG C, and pH is 6~10, and sedimentation time is 1~60min;
(4) in potentiostatic electrodeposition CoS nano-chip arrays, graphene oxide is electrochemically reduced to Graphene, forms Graphene-CoS nanometer sheet laminated film.
Preferably, in described step (2), thiocarbamide/thioacetamide and cobalt chloride/cobaltous sulfate molar concentration rate are 3:1~10:1.
Preferably, in described step (3), in three electrode electro-deposition systems, work electrode is graphene oxide film, is platinum electrode to electrode, and reference electrode is saturated calomel electrode, and current potential used is-0.9~-0.8V.
Beneficial effect: a kind of Graphene-CoS nanometer sheet of used by dye sensitization solar battery provided by the invention combined counter electrode and preparation method thereof, compared with the single nanostructure form of CoS or existing Graphene-CoS combined counter electrode, there is following characteristics: combined counter electrode of the present invention has low-temperature operation, rapid large-area preparation, eco-friendly advantage, by in conjunction with CoS nano-chip arrays and Graphene bi-material, Graphene-CoS nanometer sheet the combined counter electrode forming not only has the swift electron linear transmission passage of large area electron transport layer and the CoS nanometer sheet of Graphene simultaneously, also show more electrochemical catalysis active site, strengthen I3-to the catalysis characteristics of I-reduction process, effectively promote the photoelectric conversion efficiency of battery.
Brief description of the drawings
Fig. 1 is the graphene oxide film SEM picture preparing in the substrate of ITO electro-conductive glass by spraying coating process;
Fig. 2 is the SEM picture of Graphene-CoS nanometer sheet combined counter electrode of the present invention;
Fig. 3 is the XRD collection of illustrative plates of Graphene-CoS nanometer sheet combined counter electrode of the present invention, wherein abscissa be the angle of diffraction 2 θ, unit for (°), ordinate is diffracted intensity, unit is (cps);
Fig. 4 is the direct SEM picture at ITO electro-conductive glass substrate substrates CoS nanometer sheet film;
What Fig. 5 showed is the test curve that electrode is respectively to the current density-voltage (I-V) of the DSSC that Graphene (a), CoS nanometer sheet (b) and Graphene-CoS nanometer sheet compound (c) assemble, wherein abscissa is that voltage, unit are volt (V), and ordinate is that current density, unit are milliampere/square centimeter (mA/cm 2).Embodiment
Below in conjunction with example, the present invention is further described.
A kind of used by dye sensitization solar battery Graphene-CoS nanometer sheet combined counter electrode, is made up of graphene film and CoS nano-chip arrays; Described graphene film is in the substrate of ITO electro-conductive glass, to deposit graphene oxide film by spraying coating process, then through electrochemical reduction gained; Described CoS nano-chip arrays Direct Electrochemistry deposition growing is on graphene oxide film surface.The thickness of general design CoS nano-chip arrays is 0.1~2.0 μ m.
A kind of used by dye sensitization solar battery Graphene-CoS nanometer sheet combined counter electrode preparation method, first utilize Hummer's legal system for graphene oxide, ultrasonic again it is dispersed in alcohol solvent, in the substrate of ITO electro-conductive glass, deposits graphene oxide film by spraying coating process; Then taking cobalt chloride/cobaltous sulfate and thiocarbamide/thioacetamide mixed aqueous solution as electrolyte, the three electrode electro-deposition systems of the employing CoS nano-chip arrays of directly growing on graphene oxide film makes graphene oxide electrochemical reduction become Graphene simultaneously.Specifically comprise the steps:
(1) utilize Hummer's legal system for graphene oxide, the graphene oxide ethanolic solution that compound concentration is 10~50mg/L deposits graphene oxide film by spraying coating process in the substrate of ITO electro-conductive glass;
(2) thiocarbamide/thioacetamide mixed aqueous solution that cobalt chloride/cobaltous sulfate that compound concentration is 5~15mM and concentration are 15~150mM is electrolyte, and gained solution is designated as A solution; General design thiocarbamide/thioacetamide and cobalt chloride/cobaltous sulfate molar concentration rate are 3:1~10:1;
(3), taking A solution as electrolyte, adopt three electrode electro-deposition systems potentiostatic electrodeposition CoS nano-chip arrays on graphene oxide film; Electrolyte temperature is 25~55 DEG C, and pH is 6~10, and sedimentation time is 1~60min; In general design three electrode electro-deposition systems, work electrode is graphene oxide film, is platinum electrode to electrode, and reference electrode is saturated calomel electrode, and current potential used is-0.9~-0.8V;
(4) in potentiostatic electrodeposition CoS nano-chip arrays, graphene oxide is electrochemically reduced to Graphene, forms Graphene-CoS nanometer sheet laminated film, after repeatedly rinsing, is placed in baking oven dry for standby with deionized water.
Below in conjunction with embodiment, the present invention is made further instructions.
Embodiment 1
(1) the GO ethanolic solution that compound concentration is 10mg/L deposits GO film by spraying coating process in the substrate of ITO electro-conductive glass;
(2) the thiocarbamide mixed aqueous solution that the CoCl2 that compound concentration is 5mM and concentration are 15mM is electrolyte, and gained solution is designated as A solution;
(3), taking A solution as electrolyte, adopt three electrode electro-deposition systems potentiostatic electrodeposition CoS nano-chip arrays on GO film; Electrolyte temperature is 25 DEG C, and pH is 7, and sedimentation time is 5min, and sedimentation potential is-0.8V;
(4) in potentiostatic electrodeposition CoS nano-chip arrays, graphene oxide is electrochemically reduced to Graphene, forms Graphene-CoS nanometer sheet laminated film, after repeatedly rinsing, is placed in baking oven dry for standby with deionized water.
Embodiment 2
(1) the GO ethanolic solution that compound concentration is 20mg/L deposits GO film by spraying coating process in the substrate of ITO electro-conductive glass;
(2) the thiocarbamide mixed aqueous solution that the CoCl2 that compound concentration is 10mM and concentration are 50mM is electrolyte, and gained solution is designated as A solution;
(3), taking A solution as electrolyte, adopt three electrode electro-deposition systems potentiostatic electrodeposition CoS nano-chip arrays on GO film; Electrolyte temperature is 40 DEG C, and pH is 10, and sedimentation time is 30min, and sedimentation potential is-0.8V;
(4) in potentiostatic electrodeposition CoS nano-chip arrays, graphene oxide is electrochemically reduced to Graphene, forms Graphene-CoS nanometer sheet laminated film, after repeatedly rinsing, is placed in baking oven dry for standby with deionized water.
Embodiment 3
(1) the GO ethanolic solution that compound concentration is 30mg/L deposits GO film by spraying coating process in the substrate of ITO electro-conductive glass;
(2) the thioacetamide mixed aqueous solution that the CoSO4 that compound concentration is 15mM and concentration are 150mM is electrolyte, and gained solution is designated as A solution;
(3), taking A solution as electrolyte, adopt three electrode electro-deposition systems potentiostatic electrodeposition CoS nano-chip arrays on GO film; Electrolyte temperature is 50 DEG C, and pH is 7, and sedimentation time is 20min, and sedimentation potential is-0.8V;
(4) in potentiostatic electrodeposition CoS nano-chip arrays, graphene oxide is electrochemically reduced to Graphene, forms Graphene-CoS nanometer sheet laminated film, after repeatedly rinsing, is placed in baking oven dry for standby with deionized water.
Embodiment 4
(1) the GO ethanolic solution that compound concentration is 40mg/L deposits GO film by spraying coating process in the substrate of ITO electro-conductive glass;
(2) the thioacetamide mixed aqueous solution that the CoSO4 that compound concentration is 15mM and concentration are 150mM is electrolyte, and gained solution is designated as A solution;
(3), taking A solution as electrolyte, adopt three electrode electro-deposition systems potentiostatic electrodeposition CoS nano-chip arrays on GO film; Electrolyte temperature is 50 DEG C, and pH is 7, and sedimentation time is 60min, and sedimentation potential is-0.9V;
(4) in potentiostatic electrodeposition CoS nano-chip arrays, graphene oxide is electrochemically reduced to Graphene, forms Graphene-CoS nanometer sheet laminated film, after repeatedly rinsing, is placed in baking oven dry for standby with deionized water.
What Fig. 1 showed is scanning electron microscopy (SEM) photo of the GO film for preparing in the substrate of ITO electro-conductive glass by spraying coating process.What Fig. 2 showed is that Graphene is covered completely by CoS nanometer sheet at Graphene-CoS nanometer sheet laminated film SEM photo of GO film substrates growth.What Fig. 3 showed is Graphene-CoS nanometer sheet laminated film X-ray diffraction (XRD) collection of illustrative plates, has proved the formation of CoS material.Contrast as pattern and size, what Fig. 4 showed is the SEM photo of the direct CoS nanometer sheet not having the ITO electro-conductive glass substrate substrates of GO to grow, and the density that comparing result is presented at the upper CoS nanometer sheet of growing of GO is larger, and size is less.
Embodiment 5
Gained Graphene-CoS nanometer sheet combined counter electrode in embodiment 2 is assembled into DSSC and carries out the experiment of photoelectric conversion efficiency test, concrete operations and test process are as follows:
By standard TiO 2light anode is immersed in sensitization in the N719 dyestuff of 0.3mmol/L, at 60 DEG C, is incubated 1h; After sensitization, with the Surlyn heat-sealing film that thickness is 60 μ m, Graphene-CoS nanometer sheet combined counter electrode of preparation in itself and embodiment 2 is packaged into sandwich sandwich structure, sandwich of layers perfusion is containing the DHS-E23 type electrolyte of iodide ion; Adopt U.S. Oriel94022A solar simulator, at 100mW/cm 2intensity of illumination under the photoelectric conversion efficiency of test battery.What Fig. 5 showed is the test curve that electrode is respectively to the current-voltage (I-V) of the DSSC that Graphene (a), CoS nanometer sheet (b) and Graphene-CoS nanometer sheet compound (c) assemble.Result demonstration, the DSSC being assembled by Graphene-CoS nanometer sheet combined counter electrode shows higher photoelectric conversion efficiency (η=5.40%).In other embodiment that this case is enumerated, assemble DSSC by Graphene-CoS nanometer sheet combined counter electrode and all show higher photoelectric conversion efficiency.
The above is only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.

Claims (6)

1. used by dye sensitization solar battery Graphene-CoS nanometer sheet combined counter electrode, is characterized in that: described combined counter electrode is made up of graphene film and CoS nano-chip arrays; Described graphene film is in the substrate of ITO electro-conductive glass, to deposit graphene oxide film by spraying coating process, then through electrochemical reduction gained; Described CoS nano-chip arrays Direct Electrochemistry deposition growing is on graphene oxide film surface.
2. used by dye sensitization solar battery Graphene-CoS nanometer sheet combined counter electrode according to claim 1, is characterized in that: the thickness of described CoS nano-chip arrays is 0.1~2.0 μ m.
3. used by dye sensitization solar battery Graphene-CoS nanometer sheet combined counter electrode preparation method, it is characterized in that: first utilize Hummer's legal system for graphene oxide, ultrasonic again it is dispersed in alcohol solvent, in the substrate of ITO electro-conductive glass, deposits graphene oxide film by spraying coating process; Then taking cobalt chloride/cobaltous sulfate and thiocarbamide/thioacetamide mixed aqueous solution as electrolyte, the three electrode electro-deposition systems of the employing CoS nano-chip arrays of directly growing on graphene oxide film makes graphene oxide electrochemical reduction become Graphene simultaneously.
4. used by dye sensitization solar battery Graphene-CoS nanometer sheet combined counter electrode preparation method according to claim 3, is characterized in that: specifically comprise the steps:
(1) utilize Hummer's legal system for graphene oxide, the graphene oxide ethanolic solution that compound concentration is 10~50mg/L deposits graphene oxide film by spraying coating process in the substrate of ITO electro-conductive glass;
(2) thiocarbamide/thioacetamide mixed aqueous solution that cobalt chloride/cobaltous sulfate that compound concentration is 5~15mM and concentration are 15~150mM is electrolyte, and gained solution is designated as A solution;
(3), taking A solution as electrolyte, adopt three electrode electro-deposition systems potentiostatic electrodeposition CoS nano-chip arrays on graphene oxide film; Electrolyte temperature is 25~55 DEG C, and pH is 6~10, and sedimentation time is 1~60min;
(4) in potentiostatic electrodeposition CoS nano-chip arrays, graphene oxide is electrochemically reduced to Graphene, forms Graphene-CoS nanometer sheet laminated film.
5. used by dye sensitization solar battery Graphene-CoS nanometer sheet combined counter electrode preparation method according to claim 4, it is characterized in that: in described step (2), thiocarbamide/thioacetamide and cobalt chloride/cobaltous sulfate molar concentration rate are 3:1~10:1.
6. used by dye sensitization solar battery Graphene-CoS nanometer sheet combined counter electrode preparation method according to claim 4, it is characterized in that: in described step (3), in three electrode electro-deposition systems, work electrode is graphene oxide film, be platinum electrode to electrode, reference electrode is saturated calomel electrode, and current potential used is-0.9~-0.8V.
CN201410211259.0A 2014-05-19 2014-05-19 Graphene-CoS nanosheet composite counter electrode and preparation method thereof Pending CN103985546A (en)

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CN104399494A (en) * 2014-12-10 2015-03-11 吉林大学 Carbon-coated cobalt sulfide material as well as preparing method thereof and application of carbon-coated cobalt sulfide material in aspect of water cracking hydrogen production
CN105405663A (en) * 2015-10-30 2016-03-16 东南大学 Electrochemical preparation method of MoS<2>/graphene composite counter electrode
CN106841614A (en) * 2017-01-19 2017-06-13 济南大学 It is a kind of while with the preparation and application of two methods checking type immunosensor mutually
CN107731537A (en) * 2017-09-28 2018-02-23 安徽大学 A kind of Co3S4Ultrathin nanometer piece/rGO composite constructions, preparation method and application
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CN110479275A (en) * 2019-07-23 2019-11-22 华东师范大学 A kind of preparation and its application loading super-small composite Nano catalysis material device

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CN104399494A (en) * 2014-12-10 2015-03-11 吉林大学 Carbon-coated cobalt sulfide material as well as preparing method thereof and application of carbon-coated cobalt sulfide material in aspect of water cracking hydrogen production
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CN106841614A (en) * 2017-01-19 2017-06-13 济南大学 It is a kind of while with the preparation and application of two methods checking type immunosensor mutually
CN107731537A (en) * 2017-09-28 2018-02-23 安徽大学 A kind of Co3S4Ultrathin nanometer piece/rGO composite constructions, preparation method and application
CN109036864A (en) * 2018-07-26 2018-12-18 常州工学院 A kind of preparation method and application of nano nickel sulphide-graphene combination electrode material
CN109036864B (en) * 2018-07-26 2020-12-01 常州工学院 Preparation method and application of nano nickel sulfide-graphene composite electrode material
CN110479275A (en) * 2019-07-23 2019-11-22 华东师范大学 A kind of preparation and its application loading super-small composite Nano catalysis material device

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Application publication date: 20140813