CN104900414A - Method for preparing carbon film counter electrode for dye-sensitized solar cell - Google Patents
Method for preparing carbon film counter electrode for dye-sensitized solar cell Download PDFInfo
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- CN104900414A CN104900414A CN201510277543.2A CN201510277543A CN104900414A CN 104900414 A CN104900414 A CN 104900414A CN 201510277543 A CN201510277543 A CN 201510277543A CN 104900414 A CN104900414 A CN 104900414A
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- Y02E10/542—Dye sensitized solar cells
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Abstract
A method for preparing a carbon film counter electrode for a dye-sensitized solar cell includes uniformly mixing water soluble carbon precursor and water with a mass ratio of 1: (1.5-3), adding acetylacetone and acetone, uniformly stirring to obtain a mixed solution, depositing the mixed solution on a conductive substrate through spin coating or spraying method, insulating for 0.5-2 h under a temperature of 60-100 DEG C, insulting the deposited conductive substrate for 0.5-2 h under a temperature of 500 DEG C, and cooling in furnace to room temperature afterwards, to obtain the carbon film counter electrode for the dye-sensitized solar cell. The method prevents use of a binder, overcomes the defect that loose powdered carbon may easily fall off the conductive substrate in the prior art. The intact outer macroscopic structure of a carbon film is formed, and an effective channel for introducing electrons of external circuits is provided. Electron losses due to usage of binders can be prevented, and the electrons of external circuits can be transmitted to the surface of the carbon film faster to participate in electrolyte reduction.
Description
Technical field
The present invention relates to energy conversion and technical field of memory, particularly a kind of C film for dye-sensitized solar cells is to the preparation method of electrode.
Background technology
Dye-sensitized solar cells is as a class novel thin film solar cell, except there is higher conversion efficiency, (be stabilized in 10%), also there is the feature that crystal-silicon solar cell does not possess: cost lower (being about the 1/5-1/10 of crystal-silicon solar cell), technique are simple, device can translucentization etc.Typical dye-sensitized solar cells is by light anode, sensitizer, electrolyte, form electrode four part, wherein electrode is made up of electro-conductive glass and the platinum catalysis layer that deposits its surface, plays and collect from outside electronics and the electrolytical key player of catalytic reduction.But the use of platinum not only increases the cost of device, and be easily corroded in the electrolyte because soaking for a long time, and then affect stability.Therefore, the development of non-platinum catalysis layer is one of key issue faced in propelling dye-sensitized solar cells industrialization process.
In numerous non-platinum catalysis layer materials, low cost, high catalytic activity and the material with carbon element of wide material sources has application potential.The material with carbon element used as Catalytic Layer comprises graphite, active carbon, carbon black, fullerene, carbon nano-tube, Graphene and porous carbon etc., can application reference number be the Chinese invention patent " a kind of high hole carbon back combined counter electrode for dye-sensitized solar cells and preparation method thereof " of CN201110179512, can also application reference number be that " the flexible carbon of DSSC is to the preparation method of electrode for the Chinese invention patent of CN201310213532, flexible carbon is to electrode and battery " and application number be the Chinese invention patent " in DSSC, carbon is to the preparation method of electrode " of CN201210094885.But carbon is still a problem needing to be solved further to the long-time stability of electrode.Bulk carbon particle is the main cause causing stability to decline from coming off conductive substrates, trace sth. to its source and be that adopted Catalytic Layer is by powder carbon material molding bonded (Lee WJ, Ramasamy E, Lee DY, et al.Performance variation of carbon counter electrode based dye-sensitized solar cell.Sol Energy Mater Sol Cells, 2008,92 (7): 814-818; Lee WJ, Ramasamy E, Lee DY, et al.Grid type dye-sensitized solar cell module with carbon counter electrode.J Photoch Photobio A, 2008,194 (1): 27-30).
Summary of the invention
For above-mentioned defect of the prior art or deficiency, the object of the present invention is to provide a kind of carbon Catalytic Layer to have growth in situ and form complete external macrostructure and the C film for dye-sensitized solar cells of binder free to the preparation method of electrode.
For achieving the above object, the technical solution used in the present invention is:
For the C film of dye-sensitized solar cells to a preparation method for electrode, comprise the following steps:
1) prepare burden:
According to mass ratio 1:(1.5 ~ 3), water-soluble carbonaceous presoma and water are mixed, then adds acetylacetone,2,4-pentanedione and acetone, after stirring, obtain mixed solution; Wherein, the addition of acetylacetone,2,4-pentanedione is 20 ~ 50% of water-soluble carbonaceous presoma weight, and the addition of acetone is 20 ~ 50% of water-soluble carbonaceous presoma weight;
2) coating:
Adopt spin-coating method or spraying process to be deposited in conductive substrates by mixed solution, then at 60 ~ 100 DEG C, be incubated 0.5 ~ 2h;
3) pyrolysis:
By the conductive substrates after coating under argon gas or nitrogen protection, in 500 DEG C of insulation 0.5 ~ 2h, cool to less than 150 DEG C subsequently with the furnace, obtain C film for dye-sensitized solar cells to electrode.
Described water-soluble carbonaceous presoma is the mixture of one or more arbitrary proportions in ethylene glycol, polyethylene glycol, water soluble starch, fructose, glucose.
The molecular weight of described polyethylene glycol is between 200 ~ 20000.
Described stirring is at room temperature carried out, and the time of stirring is 20-60min.
Described step 2) in insulation carry out in air atmosphere.
Described conductive substrates is FTO electro-conductive glass, ITO electro-conductive glass or AZO electro-conductive glass.
Described 500 DEG C is carry out heating up reaching with the heating rate of 2 ~ 5 DEG C/min from room temperature.
Compared with the prior art, beneficial effect of the present invention is:
The present invention for predominant starting material with water-soluble carbonaceous presoma and water, obtains C film to electrode through batching, coating, pyrolysis three operations, has the features such as raw material is extensive and cheap, preparation technology simple, production equipment requirement is low.Particularly in pyrolysis phase, the crosslinked shape water-soluble carbonaceous precursor in situ being attached to conductive substrates surface is converted into the C film (i.e. carbon Catalytic Layer) with complete external macrostructure, not only avoid use binding agent, and to overcome in prior art bulk carbon powder easily from the deficiency that conductive substrates comes off.The C film of the complete external macrostructure in the application also provides effective passage for external circuit electronics imports simultaneously, avoid the loss of electrons using binding agent to cause, make external circuit electronics be transferred to carbon film surface more quickly and then participate in electrolyte reduction.In addition, the C film that the present invention obtains has higher visible light transmittance rate to electrode, transmitance in 400 ~ 700nm visible-range can arrive about 75%, for translucentization of corresponding dye-sensitized solar cells provides guarantee, is conducive to BIPV.The present invention also can be applicable to the energy storage such as lithium battery, ultracapacitor field.
Accompanying drawing explanation
Fig. 1 be in the embodiment of the present invention 1 C film to the photomacrograph of electrode;
Fig. 2 be in the embodiment of the present invention 1 C film to the OM pattern (× 200) of electrode;
Fig. 3 is the light transmittance curve of C film of the present invention to electrode;
Fig. 4 is the stability curve of C film of the present invention to the dye-sensitized solar cells that electrode builds;
Fig. 5 be in the embodiment of the present invention 2 C film to the OM pattern (× 200) of electrode;
Fig. 6 be in the embodiment of the present invention 3 C film to the OM pattern (× 200) of electrode.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in detail.
Embodiment 1:
1) prepare burden:
Be 1:2 according to mass ratio, at room temperature 30min is stirred by after water-soluble carbonaceous presoma and water mixing, then add the acetylacetone,2,4-pentanedione of water-soluble carbonaceous presoma weight 24% and the acetone of water-soluble carbonaceous presoma weight 39%, more at room temperature stir 30min, obtain mixed solution;
2) coating:
Adopt spin-coating method to be deposited in conductive substrates by mixed solution, and at 60 DEG C, be incubated 2h in air atmosphere;
3) pyrolysis:
By the conductive substrates after coating under nitrogen protection, rise to 500 DEG C from room temperature with the heating rate of 5 DEG C/min and be incubated 2h, then cooling to less than 150 DEG C with the furnace, finally stop air feed, obtaining C film for dye-sensitized solar cells to electrode.
Described water-soluble carbonaceous presoma is ethylene glycol.
Described conductive substrates is FTO electro-conductive glass.
The C film that the present embodiment obtains to the photomacrograph of electrode and OM pattern respectively see Fig. 1 and Fig. 2.C film has excellent visible light-transmissive performance to electrode as can be seen from Figure 1; The carbon Catalytic Layer being attached to conductive substrates as can be seen from Figure 2 has complete external macrostructure, without any crackle; C film is to the transmitance of electrode in 400 ~ 700nm visible-range all about 75%, and corresponding light transmittance curve is see Fig. 3.The C film that the present embodiment obtains is used for dye-sensitized solar cells to electrode.There is not obvious decline in the relative efficiency of dye-sensitized solar cells, corresponding stability curve is see Fig. 4 in 500h.
Embodiment 2:
1) prepare burden:
Be 1:2 according to mass ratio, at room temperature 30min is stirred by after water-soluble carbonaceous presoma and water mixing, then add the acetylacetone,2,4-pentanedione of water-soluble carbonaceous presoma weight 24% and the acetone of water-soluble carbonaceous presoma weight 39%, more at room temperature stir 30min, obtain mixed solution;
2) coating:
Adopt spin-coating method to be deposited in conductive substrates by mixed solution, and at 60 DEG C, be incubated 2h in air atmosphere;
3) pyrolysis:
By the conductive substrates after coating under nitrogen protection, rise to 500 DEG C from room temperature with the heating rate of 2 DEG C/min and be incubated 0.5h, then cooling to less than 150 DEG C with the furnace, finally stop air feed, obtaining C film for dye-sensitized solar cells to electrode.
Described water-soluble carbonaceous presoma is water soluble starch.
Described conductive substrates is FTO electro-conductive glass.
The present embodiment obtain C film to the OM pattern of electrode see Fig. 5.The carbon Catalytic Layer being attached to conductive substrates as can be seen from Figure 5 has complete external macrostructure, without any crackle; C film is to the transmitance of electrode in 400 ~ 700nm visible-range substantially higher than 20%, and corresponding light transmittance curve is see Fig. 3.The C film that the present embodiment obtains is used for dye-sensitized solar cells to electrode.There is not obvious decline in the relative efficiency of dye-sensitized solar cells, corresponding stability curve is see Fig. 4 in 500h.
Embodiment 3:
1) prepare burden:
Be 1:1.5 according to mass ratio, at room temperature 30min is stirred by after water-soluble carbonaceous presoma and water mixing, then add the acetylacetone,2,4-pentanedione of water-soluble carbonaceous presoma weight 30% and the acetone of water-soluble carbonaceous presoma weight 50%, more at room temperature stir 30min, obtain mixed solution;
2) coating:
Adopt spin-coating method to be deposited in conductive substrates by mixed solution, and at 100 DEG C, be incubated 0.5h in air atmosphere;
3) pyrolysis:
By the conductive substrates after coating under argon shield, rise to 500 DEG C from room temperature with the heating rate of 5 DEG C/min and be incubated 0.5h, then cooling to less than 150 DEG C with the furnace, finally stop air feed, obtaining C film for dye-sensitized solar cells to electrode.
Described water-soluble carbonaceous presoma is polyethylene glycol-800.
Described conductive substrates is ITO electro-conductive glass.
The present embodiment obtain C film to the OM pattern of electrode see Fig. 6.The carbon Catalytic Layer being attached to conductive substrates as can be seen from Figure 6 has complete external macrostructure, without any crackle; C film is to the transmitance of electrode in 400 ~ 700nm visible-range all about 75%, and corresponding light transmittance curve is see Fig. 3.The C film that the present embodiment obtains is used for dye-sensitized solar cells to electrode.There is not obvious decline in the relative efficiency of dye-sensitized solar cells, corresponding stability curve is see Fig. 4 in 500h.
Embodiment 4
1) prepare burden:
Be 1:3 according to mass ratio, at room temperature 30min is stirred by after water-soluble carbonaceous presoma and water mixing, then add the acetylacetone,2,4-pentanedione of water-soluble carbonaceous presoma weight 20% and the acetone of water-soluble carbonaceous presoma weight 45%, more at room temperature stir 20min, obtain mixed solution;
2) coating:
Adopt spraying process to be deposited in conductive substrates by mixed solution, and at 80 DEG C, be incubated 1h in air atmosphere;
3) pyrolysis:
By the conductive substrates after coating under nitrogen protection, rise to 500 DEG C from room temperature with the heating rate of 3 DEG C/min and be incubated 2h, then cooling to less than 150 DEG C with the furnace, finally stop air feed, obtaining C film for dye-sensitized solar cells to electrode.
Described water-soluble carbonaceous presoma is the fructose of arbitrary proportion and the mixture of glucose.
Described conductive substrates is FTO electro-conductive glass.
Embodiment 5
1) prepare burden:
Be 1:2.5 according to mass ratio, at room temperature 30min is stirred by after water-soluble carbonaceous presoma and water mixing, then add the acetylacetone,2,4-pentanedione of water-soluble carbonaceous presoma weight 40% and the acetone of water-soluble carbonaceous presoma weight 20%, more at room temperature stir 60min, obtain mixed solution;
2) coating:
Adopt spraying process to be deposited in conductive substrates by mixed solution, and at 90 DEG C, be incubated 0.5h in air atmosphere;
3) pyrolysis:
By the conductive substrates after insulation under nitrogen protection, rise to 500 DEG C from room temperature with the heating rate of 4 DEG C/min and be incubated 2h, then cooling to less than 150 DEG C with the furnace, finally stop air feed, obtaining C film for dye-sensitized solar cells to electrode.
Described water-soluble carbonaceous presoma is the mixture of ethylene glycol 20000 and water soluble starch arbitrary proportion.
Described conductive substrates is ITO electro-conductive glass.
Embodiment 6
1) prepare burden:
Be 1:1.8 according to mass ratio, at room temperature 30min is stirred by after water-soluble carbonaceous presoma and water mixing, then add the acetylacetone,2,4-pentanedione of water-soluble carbonaceous presoma weight 50% and the acetone of water-soluble carbonaceous presoma weight 30%, more at room temperature stir 50min, obtain mixed solution;
2) coating:
Adopt spin-coating method to be deposited in conductive substrates by mixed solution, and at 70 DEG C, be incubated 1.5h in air atmosphere;
3) pyrolysis:
By the conductive substrates after coating under argon shield, rise to 500 DEG C from room temperature with the heating rate of 5 DEG C/min and be incubated 2h, then cooling to less than 150 DEG C with the furnace, finally stop air feed, obtaining C film for dye-sensitized solar cells to electrode.
Described water-soluble carbonaceous presoma is the mixture of ethylene glycol 10000, water soluble starch and glucose arbitrary proportion.
Described conductive substrates is AZO electro-conductive glass.
The present invention for predominant starting material, obtains C film to electrode through batching, coating, the large operation of pyrolysis three with water-soluble carbonaceous presoma and water.In pyrolysis phase, the crosslinked shape water-soluble carbonaceous precursor in situ being attached to conductive substrates surface is converted into the C film (i.e. carbon Catalytic Layer) with complete external macrostructure, not only avoid binding agent to the use in electrode, and overcome bulk carbon powder that prior art brings easily from the deficiency that conductive substrates comes off.The C film of complete external macrostructure also provides effective passage for external circuit electronics imports simultaneously, avoids the loss of electrons that binding agent causes.In addition, the C film that the present invention obtains has higher visible light transmittance rate to electrode, for translucentization of corresponding dye-sensitized solar cells provides guarantee.The present invention also can be applicable to the energy storage such as lithium battery, ultracapacitor field.
Claims (7)
1. for the C film of dye-sensitized solar cells to a preparation method for electrode, it is characterized in that, comprise the following steps:
1) prepare burden:
According to mass ratio 1:(1.5 ~ 3), water-soluble carbonaceous presoma and water are mixed, then adds acetylacetone,2,4-pentanedione and acetone, after stirring, obtain mixed solution; Wherein, the addition of acetylacetone,2,4-pentanedione is 20 ~ 50% of water-soluble carbonaceous presoma weight, and the addition of acetone is 20 ~ 50% of water-soluble carbonaceous presoma weight;
2) coating:
Adopt spin-coating method or spraying process to be deposited in conductive substrates by mixed solution, then at 60 ~ 100 DEG C, be incubated 0.5 ~ 2h;
3) pyrolysis:
By the conductive substrates after coating under argon gas or nitrogen protection, in 500 DEG C of insulation 0.5 ~ 2h, cool to less than 150 DEG C subsequently with the furnace, obtain C film for dye-sensitized solar cells to electrode.
2. the C film for dye-sensitized solar cells according to claim 1 is to the preparation method of electrode, it is characterized in that: described water-soluble carbonaceous presoma is the mixture of one or more arbitrary proportions in ethylene glycol, polyethylene glycol, water soluble starch, fructose, glucose.
3. the C film for dye-sensitized solar cells according to claim 2 is to the preparation method of electrode, it is characterized in that: the molecular weight of described polyethylene glycol is between 200 ~ 20000.
4. the C film for dye-sensitized solar cells according to claim 1 is to the preparation method of electrode, it is characterized in that: described stirring is at room temperature carried out, and the time of stirring is 20 ~ 60min.
5. the C film for dye-sensitized solar cells according to claim 1 is to the preparation method of electrode, it is characterized in that: described step 2) in insulation carry out in air atmosphere.
6. the C film for dye-sensitized solar cells according to claim 1 is to the preparation method of electrode, it is characterized in that: described conductive substrates is FTO electro-conductive glass, ITO electro-conductive glass or AZO electro-conductive glass.
7. the C film for dye-sensitized solar cells according to claim 1 is to the preparation method of electrode, it is characterized in that: described 500 DEG C is carry out heating up reaching with the heating rate of 2 ~ 5 DEG C/min from room temperature.
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Citations (1)
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| CN103280319A (en) * | 2013-05-06 | 2013-09-04 | 武汉大学 | Preparation method of transparent carbon electrode in dye sensitization solar battery |
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| CN103280319A (en) * | 2013-05-06 | 2013-09-04 | 武汉大学 | Preparation method of transparent carbon electrode in dye sensitization solar battery |
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Application publication date: 20150909 |