CN101740237A - Method for preparing carbon nanotube counter electrode for dye-sensitized solar cell - Google Patents
Method for preparing carbon nanotube counter electrode for dye-sensitized solar cell Download PDFInfo
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- CN101740237A CN101740237A CN200810227107A CN200810227107A CN101740237A CN 101740237 A CN101740237 A CN 101740237A CN 200810227107 A CN200810227107 A CN 200810227107A CN 200810227107 A CN200810227107 A CN 200810227107A CN 101740237 A CN101740237 A CN 101740237A
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/542—Dye sensitized solar cells
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a method for preparing a carbon nanotube (CNT) counter electrode for a dye-sensitized solar cell. The method comprises the following steps: 1) manufacturing a film containing a catalyst on a carbon substrate, placing the carbon substrate in a reaction chamber to exhaust air in the carbon substrate, heating a specimen stage to 500 to 1,000 DEG C, wherein the catalyst at least comprises one of Fe, Co and Ni; 2) introducing carbon source gas and protective gas, wherein the flow of the carbon source gas is between 1 and 100 normal state milliliter/minute, and the flow of the protective gas is 150 normal state milliliter/minute; and maintaining the mixture for 5 to 500 minutes under plasma lighting up; 3) closing the carbon source gas, and stop lighting up and heating; and 4) cooling the reaction chamber to room temperature, and closing the protective gas. The method reinforces the adhesive force of the catalyst on the substrate so as to firmly combine a CNT growing by being induced by the catalyst with the substrate, so that the prepared carbon nanotube counter electrode is more suitable for assembly and transportation of flexible cells.
Description
Technical field
The present invention relates to field of dye-sensitized solar cells, particularly a kind of preparation method who is used for the carbon nano-tube of DSSC to electrode.
Background technology
DSSC comprises electric anode, to electrode and electrolyte.Wherein, battery is that resistance is low for the requirement to electrode, the corrosivity of catalytic activity height and electrolyte resistance.Usually, electrode is made up of substrate and catalytic active layer two parts, traditional DSSC is the electro-conductive glass that carries platinum to the electrode employing, and it has not only increased battery cost and weight, and can not be applied in the flexible battery.Carbon is as a kind of reserves height, and low-cost material has conductivity and electrochemical catalysis activity and corrosion resistance preferably, is a kind of desirable to the electrode substitution material.
Prepare in the method for carbon nano-tube to electrode existing, disclose among the CN1868869 a kind of with Ni powder and S powder spreading the method for carbon nano-tube (CNT) on carbon cloth, the inventor's mentions the employing silk-screen in first to file 200810118071.6 in addition, methods such as blade coating directly are coated in the carbon pastes of making on the carbon substrate, through processing modes such as heating the non-carbon component in the slurry is removed then, thereby obtained carbon nano-tube electrode.Yet all not tight by combining between the resulting material with carbon element of this said method and the substrate, the carbon film mechanical performance is poor, therefore easily comes off in assembling and transportation flexible battery process, is not suitable for using in practice.
Summary of the invention
The objective of the invention is to overcome the defective that exists in the above-mentioned prior art, the preparation method of the compact carbon nano-tube of a kind of material with carbon element and substrate to electrode is provided.
The objective of the invention is to be achieved through the following technical solutions:
According to an aspect of the present invention, provide a kind of preparation method who is used for the carbon nano-tube of DSSC to electrode, may further comprise the steps:
1) on carbon substrate, make the film contain catalyst, and this carbon substrate is put into reative cell, drain air wherein, specimen heating holder to 500～1000 ℃, wherein said catalyst comprises a kind of among Fe, Co, the Ni at least;
2) feed carbon-source gas and protective gas, the carbon-source gas flow is 1～100 standard state ml/min, and shield gas flow rate is 150 standard state ml/min, keeps under plasma glow start 5～500 minutes then;
3) close carbon-source gas, and stop build-up of luminance and heating;
4) reaction chamber temperature is reduced to room temperature, close protective gas.
Wherein, the thickness of film is between 5nm～500nm, preferably between 50nm～100nm in step 1); Carbon substrate is membranaceous, sheet or tabular material with carbon element, and the face resistance of this material with carbon element is between 0.01～100 Ω/, and surface density is at 0.001～0.5g/cm
2Between, thickness is between 0.05mm～5mm.
In technique scheme, described step 1) comprises:
11) colloidal sol that will contain the catalyst precursor is coated on the described carbon substrate, forms the film that contains the catalyst precursor;
12) will be covered with the described carbon substrate heated oxide in air that contains the film of catalyst precursor;
13) carbon substrate after the step 12) oxidation is put into reative cell, drain air wherein, specimen heating holder to 500～1000 ℃ feed H
2And protective gas, H
2Flow is 1～100 standard state ml/min, and shield gas flow rate is 150 standard state ml/min, under plasma glow start, keep 1～60 minute then after, close H
2
Wherein, contain that the cationic concentration of catalyst is 0.05～0.1M in the colloidal sol of catalyst precursor; The temperature of heated oxide is between 500～800 ℃.
In technique scheme, described step 11) comprises:
111) preparation contains the colloidal sol of catalyst precursor;
112) evenly dripping the described colloidal sol of step 11) on the described carbon substrate surface, spin coating is to form the film that contains the catalyst precursor on described carbon substrate surface then.
According to another aspect of the present invention, provide the carbon nano-tube of one of above technical scheme of a kind of basis acquisition to electrode.
In the present invention, catalyst Fe closely attached in the substrate, directly grows out CNT as the active site of CNT growth from substrate, strengthened the binding ability between CNT and the substrate.Therefore the invention has the beneficial effects as follows:
1. on carbon substrate, apply the film that contains catalyst, strengthened catalyst at suprabasil adhesive force, thereby the CNT by catalyst inducement growth is firmly combined with substrate, make prepared carbon nano-tube be more suitable for assembling and transportation in flexible battery to electrode.
2. utilize plasma oxide to be reduced and the CNT that grows, growth temperature is lower, and technology is easy to control, and the CNT array structure that is obtained helps the transport of electronics in film.
Description of drawings
Below, describe embodiments of the invention in conjunction with the accompanying drawings in detail, wherein:
Fig. 1 is a carbon nano-tube prepared according to the methods of the invention stereoscan photograph to electrode;
Fig. 2 is a carbon nano-tube prepared according to the methods of the invention stereoscan photograph to electrode cross-section.
Embodiment
[embodiment 1]:
1) the ferric nitrate solid (Fe (NO of weighing certain mass
3)
39H
2O) and citric acid 2g, mix and add 10mlH
2O makes it to dissolve fully; Adding an amount of ethanol and 2g polyethylene glycol then, to make overall solution volume be 50mL, stirs that to form the colloidal sol that contains catalyst precursor in one hour stand-by, wherein Fe in the colloidal sol
3+Concentration is 0.05M (mol/L);
2) get graphite paper, face resistance 7.33 * 10
-2Ω/, surface density 0.03g/cm
2, thickness is 0.1mm, and it is cleaned up, flatten with tablet press machine, evenly drip in its surface and go up the above-mentioned colloidal sol that contains catalyst precursor, on sol evenning machine with 2000 rev/mins of even glue 30 seconds, thereby form the film that thickness is approximately 50nm on the graphite paper surface;
3) with step 2) graphite paper heated oxide in air of the overlay film of gained, temperature is 400 ℃, temperature retention time is 30 minutes, to form Fe in film
2O
3And the organic substance in the removal film;
4) then the graphite paper after the step 3) oxidation is put into chemical vapor deposition (CVD) reative cell, detected the device air-tightness intact after, open aspiration pump, drain the air in the reative cell; After air to be confirmed drained, specimen heating holder to 600 ℃ fed H
2And N
2, flow is respectively 6sccm (standard state ml/min) and 150sccm, regulates to make the reative cell stable gas pressure, opens microwave power supply, the build-up of luminance plasma, and make microwave reflection power drop to zero; After reduction in 5 minutes, the Fe in the film
2O
3Be reduced, form metallic catalyst Fe, close H
2
5) feed methane, flow is 100sccm, regulates microwave power and reative cell air pressure, keeps 5 minutes CNT growth times;
6) close methane, microwave and radio frequency heating source successively;
7) the question response room temperature is reduced to room temperature, closes N
2, taking out sample, the black film of graphite paper and top one deck even compact thereof then is that carbon nano-tube of the present invention is to electrode.
Fig. 1 and Fig. 2 are respectively that carbon nano-tube prepared according to the methods of the invention is to the stereoscan photograph of electrode and the stereoscan photograph of cross section thereof.As can be seen from the figure, CNT directly grows out from graphite paper, form the CNT array structure, this structure helps the transport of electronics in film, therefore help the raising of battery performance, in addition, carbon nano-tube is many walls CNT, between 10nm～100nm, the thickness of carbon nanotube layer is greatly about about 10 μ m greatly in the caliber distribution.
The colloidal sol that contains the catalyst precursor that the only exemplary centrifugal whirl coating technology of employing of the present invention will prepare is coated in and forms film in the substrate, process through heated oxide, reduction obtains catalyst then, be appreciated that other can transfer to the colloidal sol that contains the catalyst precursor in the substrate and the method that forms film also can be used at this, such as silk screen printing, blade coating, lift, impregnating.
The distortion of the another kind of present embodiment is directly to make the film that contains catalyst in substrate, utilizes the plasma CNT that grows on the carbon substrate surface of the film that is covered with catalyst then.For those skilled in the art will appreciate that this distortion directly forms the film that contains metallic catalyst on carbon substrate, thereby omitted above-mentioned process of joining glue, gluing, oxidation, reduction, but this method still can realize purpose of the present invention.Said method can may further comprise the steps after being out of shape:
1) on carbon substrate, make the film contain catalyst, and this carbon substrate put into reative cell, has detected the device air-tightness intact after, the unlatching aspiration pump drains air wherein; After air to be confirmed drains, specimen heating holder to 600 ℃;
2) feed methane and N
2, flow is respectively 100sccm and 150sccm, regulates to make the reative cell stable gas pressure, opens microwave power supply, the build-up of luminance plasma, and make microwave reflection power drop to zero, keep 5 minutes CNT growth times;
3) close methane, microwave and radio frequency heating source successively;
4) the question response room temperature is reduced to room temperature, closes N
2, taking out sample, the black film of graphite paper and top one deck even compact thereof then is that carbon nano-tube of the present invention is to electrode.
Known method of making film in substrate comprises sputter coating, ion film plating, chemical vapour deposition (CVD), solution plated film etc., by having adhesive force preferably between prepared film of said method and the substrate.
With the invention described above be covered with CNT electrode is adopted document Journal of the AmericanChemical Society, vol.115, p.6382, method in 1993 is assembled into DSSC, and detailed process is as follows: the method depositing Ti O that passes through blade coating or silk screen printing on electro-conductive glass
2Film is at 450 ℃ of annealing 30 minutes, Using such method depositing Ti O
2Film 2～5 times makes film thickness be about 10～20 microns; Annealed 30 minutes for 450 ℃ then, when being cooled to about 80 ℃, TiO
2Film steeps into dyestuff RuL
2(NCS)
2.2H
2O (wherein, L be 2,2 '-bipyridine-4,4 '-dicarboxylic acids) ethanolic solution in (concentration 0.3mM); After soaking 12 hours, slide is taken out, dry under nitrogen, then this slide is as the light anode of DSSC.Negative electrode is that the prepared carbon nano-tube of the present invention is to electrode.It between anode and the negative electrode electrolyte.Under simulated solar irradiation, measure the current-voltage curve of the solar cell that assembles, and calculate its peak power output (electric current and voltage maximum product).This peak power output value then is the efficient of battery with the ratio of input light intensity, and promptly luminous energy is converted into the efficient of electric energy, and the battery efficiency that records the battery of being assembled by embodiment 1 is 4.3%.
For a person skilled in the art, should be appreciated that graphite paper among the present invention only for exemplary, can use other carbon substrate, such as membranaceous, sheet or tabular material with carbon element, the face resistance of this material with carbon element is between 0.01-100 Ω/, and mass area ratio is at 0.001～0.5g/cm
2Between, thickness is between 0.05mm～5mm; Further, material with carbon element can be flexible graphite paper, carbon fiber paper, carbon plate or carbon plate.In addition, in other embodiments, can be with N
2Replace with protective gas commonly used such as Ar gas, He gas; Methane is to be used to provide growth CNT required carbon source, therefore can also use carbon-source gas such as ethane, ethene to substitute in other embodiments.
[embodiment 2～76]:
With reference to the preparation condition in the table 1, realize embodiment 2～76 according to the method identical with embodiment 1.And, the method that is adopted by embodiment 1 is assembled into DSSC with embodiment 2～76 resulting carbon nano-tube to electrode, and the battery efficiency (seeing Table 1) of testing them, the result shows: under the same test condition, most of carbon nano-tube of the present invention has the battery efficiency close with traditional platinum electrode to electrode, the battery efficiency of graphite paper carbon nano-tube power cell of wherein utilizing the embodiment of the invention 3 preparation further specifies the beneficial effect of carbon nano-tube of the present invention to electrode than the height (seeing Table 2) of pyrolysis platinum.
The preparation condition of table 1 embodiment of the invention and battery efficiency
(in the table 1: a represent flexible graphite paper (2.5mm is thick, face resistance 0.1 Ω/, surface density is at 0.2g/cm
2); B represent flexible graphite paper (5mm is thick, face resistance 0.1 Ω/, surface density is at 0.5g/cm
2); C represent carbon fiber paper (0.05mm is thick, face resistance 30 Ω/, surface density is at 0.001g/cm
2); D represent carbon fiber paper (5mm is thick, face resistance 0.3 Ω/, surface density is at 0.5g/cm
2)
The comparison of table 2. optimization graphite paper carbon nano-tube power cell performance and pyrolysis platinum battery performance
As can be seen from Table 1, contain that the cationic concentration of catalyst is 0.05～0.1M in the colloidal sol of catalyst precursor; The thickness of plated film (coating film thickness herein is the thickness without the peroxidating reduction, and oxidation-reduction process can be ignored to the influence of thickness) is for 5nm～500nm, preferably between 50nm～100nm; The thickness of the layer of resulting carbon nano-tube is between 200nm-20 μ m; Resulting battery efficiency is better when using Fe as catalyst.
Although the present invention is made specific descriptions with reference to the above embodiments, but for the person of ordinary skill of the art, should be appreciated that and can make amendment or improve based on content disclosed by the invention, and these modifications and improving all within spirit of the present invention and scope.
Claims (10)
1. preparation method who is used for the carbon nano-tube of DSSC to electrode may further comprise the steps:
1) on carbon substrate, make the film contain catalyst, and this carbon substrate is put into reative cell, drain air wherein, specimen heating holder to 500～1000 ℃, wherein said catalyst comprises a kind of among Fe, Co, the Ni at least;
2) feed carbon-source gas and protective gas, the carbon-source gas flow is 1～100 standard state ml/min, and shield gas flow rate is 150 standard state ml/min, keeps under plasma glow start 5～500 minutes then;
3) close carbon-source gas, and stop build-up of luminance and heating;
4) reaction chamber temperature is reduced to room temperature, close protective gas.
2. the method for claim 1 is characterized in that, at the thickness of film described in the described step 1) between 5nm～500nm.
3. method as claimed in claim 2 is characterized in that the thickness of described film is preferably between 50nm～100nm.
4. the method for claim 1 is characterized in that, described carbon substrate is membranaceous, sheet or tabular material with carbon element, and the face resistance of described material with carbon element is between 0.01～100 Ω/, and surface density is at 0.001～0.5g/cm
2Between, thickness is between 0.05mm～5mm.
5. method as claimed in claim 4 is characterized in that, described material with carbon element is flexible graphite paper, carbon fiber paper, carbon plate or carbon plate.
6. the method for claim 1 is characterized in that, described step 1) comprises:
11) colloidal sol that will contain the catalyst precursor is coated on the described carbon substrate, forms the film that contains the catalyst precursor;
12) will be covered with the described carbon substrate heated oxide in air that contains the film of catalyst precursor;
13) carbon substrate after the step 12) oxidation is put into reative cell, drain air wherein, specimen heating holder to 500～1000 ℃ feed H
2And protective gas, H
2Flow is 1～100 standard state ml/min, and shield gas flow rate is 150 standard state ml/min, under plasma glow start, keep 1～60 minute then after, close H
2
7. method as claimed in claim 6 is characterized in that, the cationic concentration of catalyst is 0.05～0.1M in the described colloidal sol that contains the catalyst precursor;
8. method as claimed in claim 6 is characterized in that the temperature of described heated oxide is between 500～800 ℃.
9. method as claimed in claim 6 is characterized in that, described step 11) comprises:
111) preparation contains the colloidal sol of catalyst precursor;
112) evenly dripping the described colloidal sol of step 11) on the described carbon substrate surface, spin coating is to form the film that contains the catalyst precursor on described carbon substrate surface then.
10. a carbon nano-tube that obtains according to the described preparation method of one of claim 1 to 9 is to electrode.
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| CN101740237B CN101740237B (en) | 2012-05-23 |
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| CN102068983A (en) * | 2010-12-20 | 2011-05-25 | 宁波工程学院 | Preparation method of proton exchange membrane fuel cell catalyst |
| CN102496474A (en) * | 2011-11-12 | 2012-06-13 | 太原理工大学 | Preparation method for counter electrode of dye-sensitized solar cell |
| CN103384007A (en) * | 2013-07-23 | 2013-11-06 | 深圳清华大学研究院 | Carbon nano tube/graphene composite negative pole material, preparation method thereof and lithium battery |
| CN104485232A (en) * | 2014-12-18 | 2015-04-01 | 中国科学院上海硅酸盐研究所 | Preparing method of counter electrode for dye-sensitized solar cell |
| CN105555708A (en) * | 2013-09-30 | 2016-05-04 | 日本瑞翁株式会社 | Carbon nanotubes, dispersion liquid thereof, carbon nanotube-containing film and composition material |
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| CN100395896C (en) * | 2003-12-05 | 2008-06-18 | 鸿富锦精密工业（深圳）有限公司 | Dye sensitized solar batter and its electrode |
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| CN102068983A (en) * | 2010-12-20 | 2011-05-25 | 宁波工程学院 | Preparation method of proton exchange membrane fuel cell catalyst |
| CN102068983B (en) * | 2010-12-20 | 2012-07-18 | 宁波工程学院 | Preparation method of proton exchange membrane fuel cell catalyst |
| CN102496474A (en) * | 2011-11-12 | 2012-06-13 | 太原理工大学 | Preparation method for counter electrode of dye-sensitized solar cell |
| CN102496474B (en) * | 2011-11-12 | 2013-07-17 | 太原理工大学 | Preparation method for counter electrode of dye-sensitized solar cell |
| CN103384007A (en) * | 2013-07-23 | 2013-11-06 | 深圳清华大学研究院 | Carbon nano tube/graphene composite negative pole material, preparation method thereof and lithium battery |
| CN103384007B (en) * | 2013-07-23 | 2015-11-18 | 深圳清华大学研究院 | Carbon nano tube/graphene composite negative pole and preparation method thereof, lithium battery |
| CN105555708A (en) * | 2013-09-30 | 2016-05-04 | 日本瑞翁株式会社 | Carbon nanotubes, dispersion liquid thereof, carbon nanotube-containing film and composition material |
| CN104485232A (en) * | 2014-12-18 | 2015-04-01 | 中国科学院上海硅酸盐研究所 | Preparing method of counter electrode for dye-sensitized solar cell |
| CN104485232B (en) * | 2014-12-18 | 2017-06-06 | 中国科学院上海硅酸盐研究所 | A kind of preparation method of used by dye sensitization solar battery to electrode |
| CN105977035A (en) * | 2016-07-27 | 2016-09-28 | 杨炳 | Dye-sensitized solar cell of novel electrode structure |
| CN111681879A (en) * | 2020-07-17 | 2020-09-18 | 东北师范大学 | Non-platinum-based transparent electrode material and preparation method and application thereof |
| CN111681879B (en) * | 2020-07-17 | 2021-12-07 | 东北师范大学 | Non-platinum-based transparent electrode material and preparation method and application thereof |
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