CN102324319B - Method for preparing graphene/platinum nano counter electrode material for dye sensitized solar cell - Google Patents

Method for preparing graphene/platinum nano counter electrode material for dye sensitized solar cell Download PDF

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CN102324319B
CN102324319B CN2011101934594A CN201110193459A CN102324319B CN 102324319 B CN102324319 B CN 102324319B CN 2011101934594 A CN2011101934594 A CN 2011101934594A CN 201110193459 A CN201110193459 A CN 201110193459A CN 102324319 B CN102324319 B CN 102324319B
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CN102324319A (en
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王忠胜
宫峰
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Fudan University
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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
    • 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
    • Y02E10/549—Organic PV cells
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention belongs to the technical field of dye sensitized solar cells, in particular to a method for preparing a graphene/platinum nano counter electrode material for a dye sensitized solar cell. The method comprises the following steps of: soaking a conducting substrate on which a polyelectrolyte is adsorbed in a graphene suspension, a polyelectrolyte solution and a chloroplatinic acid solution in sequence in an electrostatic self-assembly way to form a self-assembly ultrathin film with a polyelectrolyte/graphene/polyelectrolyte/chloroplatinic acid structure on the surface of the conducting substrate under the action of electrostatic attraction; and sintering and transforming into a 'graphene/platinum nanoparticle' ultrathin film. The film can be taken as a counter electrode material for the dye sensitized solar cell. The preparation method has a simple process, the prepared counter electrode has extremely low platinum load amount, the cost of the counter electrode and the dye sensitized solar cell is greatly lowered, and the method can be applied to large-scale production of assembly line operation.

Description

The preparation method of used by dye sensitization solar battery graphene/platinum nano counter electrode material
Technical field
The invention belongs to the DSSC technical field, be specifically related to a kind of preparation method of graphene/platinum nano counter electrode material of used by dye sensitization solar battery.
Background technology
Since M. Gr professor tzel in 1991 introduces dye sensitization broad stopband TiO with the concept of nanoporous 2In the semiconducter research, obtain dye-sensitized solar cells (the dye-sensitized solar cells of energy conversion efficiency 7.1 %, DSSCs) (Nature since, 1991,353,737), DSSCs obtains rapidly international academia and industrial quarters extensive concern with its low cost, relatively simple manufacture craft, higher characteristics such as electricity conversion.
DSSCs mainly forms by the porous semi-conductor nano-crystal film of dye sensitization, electrolyte with to electrode.Dye molecule is subject to exciting after the illumination, the conduction band of electronic injection semiconductive thin film, and electronics is got back to electrode through external circuit; I -Ion is diffused into reduction-oxidation attitude dyestuff on the semiconductive thin film, makes dyestuff regeneration, I -Ion is oxidized to I 3 -Ion, the latter is obtaining electronics generation I to electrode -Ion, so circulation, thus realize opto-electronic conversion.In this process, reduce because above-mentioned reduction reaction is being very necessary to the energy consumption on the electrode.Therefore, as one of them important component part, the catalytic performance of electrode there is important impact to the electricity conversion of DSSCs.Platinum adopts magnetron sputtering (Electrochimi. Acta. usually to electrode, 2001,46,3457) and chloroplatinic acid thermal decomposition (J. Electrochem. Soc., 1997,144,876) method makes, although preferably catalysis performance and combination property are arranged, because platinum is noble metal, if having obvious limitation with these methods for large-scale production and application.Therefore reduce the platinum load capacity, and to keep catalytic activity and photovoltaic performance to electrode be a study hotspot.
Summary of the invention
What the object of the present invention is to provide that a kind of platinum load capacity is low, utilance is high is used for used by dye sensitization solar battery graphene/platinum nano particle to the preparation method of electrode material.
The preparation method of used by dye sensitization solar battery graphene/platinum nano counter electrode material provided by the invention, concrete steps are as follows:
(1) conductive substrates that cleans up is dipped in 0.1-5 h in the polyelectrolyte solution, after taking out with solvent washing, dry up;
(2) immerse again 0.1-5 h in graphene suspension or the platinum acid chloride solution;
(3) repeat above-mentioned steps (1), (2), carry out layer by layer self assembly, form (polyelectrolyte/Graphene) on the conductive substrates surface mOr (polyelectrolyte/chloroplatinic acid) nOr (polyelectrolyte/Graphene) m/ (polyelectrolyte/chloroplatinic acid) nSelf-assembling ultrathin film Deng different structure, the different numbers of plies.M, n are respectively number of repetition.General m, n are no more than 50;
(4) with above-mentioned ultrathin membrane sintering in air, temperature is 100-600 ℃, and the time is 0.1-5 h, makes it change into (Graphene) mOr (nano platinum particle) nOr (Graphene) m/ (nano platinum particle) nIsostructural ultrathin membrane.So-called ultrathin membrane, generally its thickness＜5nm.
Among the above-mentioned preparation method, described conductive substrates is the materials such as electro-conductive glass, conductive polymer membrane.
Among the above-mentioned preparation method, in the described polyelectrolyte solution, polyelectrolyte is the cationic polyelectrolytes such as diallyl dimethyl ammoniumchloride, polymine, its solvent is water, absolute ethyl alcohol, ether or acetone, or several mixed solvent wherein, the mass fraction of polyelectrolyte is 0.001-10 %, and the pH value is 6-13.Preferably: the mass fraction of polyelectrolyte is 0.1%--2 %, and the pH value is 8--10.
Among the above-mentioned preparation method, the solvent of described graphene suspension is water, absolute ethyl alcohol, DMF or dimethyl sulfoxide (DMSO), or several mixed solvent wherein, and the mass fraction of Graphene is 0.001-5 %, and the pH value is 6-13.Preferably: the mass fraction of Graphene is 0.1%--1%, and the pH value is 9--10.
Among the above-mentioned preparation method, the solvent of described platinum acid chloride solution is water, absolute ethyl alcohol, isopropyl alcohol or acetone, or several mixed solvent wherein, and the mass fraction of chloroplatinic acid is 0.001 %--20 %.The mass fraction of preferred chloroplatinic acid is 0.1 %-2 %.
Among the above-mentioned preparation method, ultrathin membrane is sintering in air, and preferred temperature is 400--600 ℃, and the time is 0.5--3h.
By prepared the having of said method (Graphene) m, (nano platinum particle) nOr (Graphene) m/ (nano platinum particle) nIsostructural ultrathin membrane can be used as used by dye sensitization solar battery to electrode material.
The thin-film material of the present invention's preparation because the specific area of metal platinum nano-particle is large, and by graphene-supported, can significantly improve catalytic effect.With this ultrathin membrane (platinum load capacity: 0.4 μ g cm -2) be used for dye-sensitized solar cells to electrode, can obtain platinum mirror with the magnetron sputtering preparation to electrode (platinum load capacity: 308.9 μ g cm -2) suitable energy conversion efficiency.Technique of the present invention is simple, and the prepared platinum load capacity to electrode is extremely low, greatly reduces the cost to electrode and even dye-sensitized solar cells, can be applicable to the large-scale production of pipelining.
Description of drawings
Fig. 1 is that the graphene/platinum nano particle of the low platinum load capacity of the present invention is to the SEM photo of electrode.
Fig. 2 is that (effective area is 0.2304 cm to the I-V curve chart of the DSSCs compare test of electrode assembling for the platinum mirror of the present invention and magnetron sputtering preparation 2).
Embodiment
Below in conjunction with specific embodiment the present invention is described in further detail.
Embodiment 1
The electro-conductive glass that cleans up is dipped in 2 h in the diallyl dimethyl ammoniumchloride aqueous solution that mass fraction is 0.5 %, water washes, dries up after taking out, immerse again mass fraction and be 2 h in the Graphene water slurry of 0.05 %, water washes, dries up after taking out, and then immerse 2 h in the above-mentioned polyelectrolyte, water washes, dries up after taking out, immerse again at last 2 h in the chloroplatinic acid aqueous solution that mass fraction is 0.05 %, water washes, dries up after taking out, and the formation structure is the self-assembling ultrathin film of polyelectrolyte/Graphene/polyelectrolyte/chloroplatinic acid.With above-mentioned ultrathin membrane 400 ℃ of sintering 1 h in air, forming structure is the ultrathin membrane of graphene/platinum nano particle.
According to conventional methods with this ultrathin membrane as electrode assembling is become DSSCs, cell area is 0.2304 cm 2Under the AM1.5 simulated solar irradiation, record current-voltage (I-V) curve (shown in Fig. 2 curve 1) of DSSC, the photovoltage that obtains opening a way ( V Oc ) be 707 mV, short-circuit photocurrent ( J Sc ) be 15.20 mA/cm 2, fill factor, curve factor ( FF) be 0.71, energy conversion efficiency ( η) be 7.63 %.
Embodiment 2
The electro-conductive glass that cleans up is dipped in 0.5 h in the diallyl dimethyl ammoniumchloride aqueous solution that mass fraction is 2 %, water washes, dries up after taking out, immerse again mass fraction and be 0.5 h in the Graphene alcohol suspension of 0.1 %, after taking out with alcohol flushing, dry up, repeat above-mentioned self assembling process 1 time, and then immerse 0.5 h in the above-mentioned polyelectrolyte, water washes, dries up after taking out, immerse again at last 0.5 h in the chloroplatinic acid aqueous solution that mass fraction is 1 %, water washes, dries up after taking out, and forming structure is (polyelectrolyte/Graphene) 2The self-assembling ultrathin film of/polyelectrolyte/chloroplatinic acid.With above-mentioned ultrathin membrane 450 ℃ of sintering 1 h in air, forming structure is (Graphene) 2The ultrathin membrane of/nano platinum particle.
According to conventional methods with this ultrathin membrane as electrode assembling is become DSSCs, cell area is 0.2304 cm 2Under the AM1.5 simulated solar irradiation, record current-voltage (I-V) curve of DSSC, the photovoltage that obtains opening a way ( V Oc ) be 713 mV, short-circuit photocurrent ( J Sc ) be 13.93 mA/cm 2, fill factor, curve factor ( FF) be 0.72, energy conversion efficiency ( η) be 7.15 %.
Embodiment 3
The electro-conductive glass that cleans up is dipped in 0.2 h in the diallyl dimethyl ammoniumchloride aqueous solution that mass fraction is 5 %, water washes, dries up after taking out, immerse again 0.2 h in the chloroplatinic acid aqueous solution that mass fraction is 1 %, water washes, dries up after taking out, and forming structure is the self-assembling ultrathin film of polyelectrolyte/chloroplatinic acid.With above-mentioned ultrathin membrane 500 ℃ of sintering 0.2 h in air, forming structure is the ultrathin membrane of nano platinum particle.
According to conventional methods with this ultrathin membrane as electrode assembling is become DSSCs, cell area is 0.2304 cm 2Under the AM1.5 simulated solar irradiation, record current-voltage (I-V) curve of DSSC, the photovoltage that obtains opening a way ( V Oc ) be 672 mV, short-circuit photocurrent ( J Sc ) be 10.12 mA/cm 2, fill factor, curve factor ( FF) be 0.68, energy conversion efficiency ( η) be 4.62 %.
Embodiment 4
The electro-conductive glass that cleans up is dipped in 0.1 h in the diallyl dimethyl ammoniumchloride aqueous solution that mass fraction is 10 %, water flushing after taking out, dry up, immerse again mass fraction and be 1 h in the Graphene alcohol suspension of 0.02 %, use alcohol flushing after taking out, dry up, and then immerse 0.1 h in the above-mentioned polyelectrolyte, water flushing after taking out, dry up, immerse again 0.5 h in the chloroplatinic acid aqueous solution that mass fraction is 0.1 %, water flushing after taking out, dry up, repeat above-mentioned Graphene self assembling process, the formation structure is the self-assembling ultrathin film of polyelectrolyte/Graphene/polyelectrolyte/chloroplatinic acid/polyelectrolyte/Graphene again.With above-mentioned ultrathin membrane 350 ℃ of sintering 2 h in air, forming structure is the ultrathin membrane of graphene/platinum nano particle/Graphene.
According to conventional methods with this ultrathin membrane as electrode assembling is become DSSCs, cell area is 0.2304 cm 2Under the AM1.5 simulated solar irradiation, record current-voltage (I-V) curve of DSSC, the photovoltage that obtains opening a way ( V Oc ) be 677 mV, short-circuit photocurrent ( J Sc ) be 8.29 mA/cm 2, fill factor, curve factor ( FF) be 0.59, energy conversion efficiency ( η) be 3.31 %.
Embodiment 5
The electro-conductive glass that cleans up is dipped in 0.5 h in the diallyl dimethyl ammoniumchloride aqueous solution that mass fraction is 5 %, water washes, dries up after taking out, immerse again mass fraction and be 0.5 h in the Graphene alcohol suspension of 0.02 %, after taking out with alcohol flushing, dry up, the formation structure is the self-assembling ultrathin film of polyelectrolyte/Graphene.Just above-mentioned ultrathin membrane is 450 ℃ of sintering 1 h in air, and forming structure is the ultrathin membrane of Graphene.
According to conventional methods with this ultrathin membrane as electrode assembling is become DSSCs, cell area is 0.2304 cm 2Under the AM1.5 simulated solar irradiation, record current-voltage (I-V) curve of DSSC, the photovoltage that obtains opening a way ( V Oc ) be 709 mV, short-circuit photocurrent ( J Sc ) be 10.64 mA/cm 2, fill factor, curve factor ( FF) be 0.25, energy conversion efficiency ( η) be 1.89 %.
Embodiment 6
The electro-conductive glass that cleans up is dipped in 1 h in the polyethyleneimine: amine aqueous solution that mass fraction is 0.5 %, water washes, dries up after taking out, immerse again mass fraction and be 1 h in the Graphene water slurry of 0.05 %, water washes, dries up after taking out, and then immerse 1 h in the above-mentioned polyelectrolyte, water washes, dries up after taking out, immerse again at last 1 h in the chloroplatinic acid aqueous solution that mass fraction is 0.05 %, water washes, dries up after taking out, and the formation structure is the self-assembling ultrathin film of polyelectrolyte/Graphene/polyelectrolyte/chloroplatinic acid.With above-mentioned ultrathin membrane 300 ℃ of sintering 5 h in air, forming structure is the ultrathin membrane of graphene/platinum nano particle.
According to conventional methods with this ultrathin membrane as electrode assembling is become DSSCs, cell area is 0.2304 cm 2Under the AM1.5 simulated solar irradiation, record current-voltage (I-V) curve of DSSC, the photovoltage that obtains opening a way ( V Oc ) be 665 mV, short-circuit photocurrent ( J Sc ) be 9.40 mA/cm 2, fill factor, curve factor ( FF) be 0.63, energy conversion efficiency ( η) be 3.94 %.
Embodiment 7
The electro-conductive glass that cleans up is dipped in 0.5 h in the polyethyleneimine: amine aqueous solution that mass fraction is 5 %, water washes, dries up after taking out, immerse again mass fraction and be 1 h in the Graphene water slurry of 0.05 %, water washes, dries up after taking out, and then immerse 0.5 h in the above-mentioned polyelectrolyte, water washes, dries up after taking out, immerse again at last 0.5 h in the chloroplatinic acid aqueous solution that mass fraction is 2 %, water washes, dries up after taking out, and the formation structure is the self-assembling ultrathin film of polyelectrolyte/Graphene/polyelectrolyte/chloroplatinic acid.With above-mentioned ultrathin membrane 500 ℃ of sintering 1 h in air, forming structure is the ultrathin membrane of graphene/platinum nano particle.
According to conventional methods with this ultrathin membrane as electrode assembling is become DSSCs, cell area is 0.2304 cm 2Under the AM1.5 simulated solar irradiation, record current-voltage (I-V) curve of DSSC, the photovoltage that obtains opening a way ( V Oc ) be 695 mV, short-circuit photocurrent ( J Sc ) be 14.74 mA/cm 2, fill factor, curve factor ( FF) be 0.71, energy conversion efficiency ( η) be 7.27 %.
Embodiment 8
The electro-conductive glass that cleans up is dipped in 0.1 h in the polyethyleneimine: amine aqueous solution that mass fraction is 15 %, water washes, dries up after taking out, immerse again mass fraction and be 0.1 h in the Graphene water slurry of 0.5 %, water washes, dries up after taking out, and then immerse 0.1 h in the above-mentioned polyelectrolyte, water washes, dries up after taking out, immerse again at last 0.1 h in the chloroplatinic acid aqueous solution that mass fraction is 5 %, water washes, dries up after taking out, and the formation structure is the self-assembling ultrathin film of polyelectrolyte/Graphene/polyelectrolyte/chloroplatinic acid.With above-mentioned ultrathin membrane 600 ℃ of sintering 0.5 h in air, forming structure is the ultrathin membrane of graphene/platinum nano particle.
According to conventional methods with this ultrathin membrane as electrode assembling is become DSSCs, cell area is 0.2304 cm 2Under the AM1.5 simulated solar irradiation, record current-voltage (I-V) curve of DSSC, the photovoltage that obtains opening a way ( V Oc ) be 713 mV, short-circuit photocurrent ( J Sc ) be 12.82 mA/cm 2, fill factor, curve factor ( FF) be 0.72, energy conversion efficiency ( η) be 6.58 %.
Comparative example 1
As a comparison, we are also in the identical situation of every other condition, the platinum mirror that adopts the magnetron sputtering method preparation to electrode assembling DSSC, under the AM1.5 simulated solar irradiation, record current-voltage (I-V) curve (shown in Fig. 2 curve 2) of DSSC, the photovoltage that obtains opening a way ( V Oc ) be 713 mV, short-circuit photocurrent ( J Sc ) be 14.80 mA/cm 2, fill factor, curve factor ( FF) be 0.76, energy conversion efficiency ( η) be 8.02 %.
According to the embodiment of the invention 1 preparation to electrode, energy conversion efficiency can reach the level suitable to electrode with the platinum mirror, illustrate that it has quite high catalytic activity, but its platinum load capacity only (is respectively 0.4 μ g cm for the nearly one thousandth of platinum mirror -2With 308.9 μ g cm -2).Manufacturing conditions of the present invention is gentle, and technique is also very simple, and the consumption of noble metal platinum is reduced greatly, thereby greatly reduces the manufacturing cost to electrode and even dye-sensitized solar cells, is expected to be applied to the large-scale production of pipelining.

Claims (5)

1. a used by dye sensitization solar battery graphene/platinum nano particle is characterized in that to the preparation method of electrode material concrete steps are as follows:
(1) conductive substrates that cleans up is dipped in 0.1-5 h in the polyelectrolyte solution, after taking out with solvent washing, dry up;
(2) immerse again 0.1-5 h in the graphene suspension;
(3) repeat above-mentioned steps (1), (2), carry out layer by layer self assembly;
(4) immerse 0.1-5 h in the polyelectrolyte solution, after taking out with solvent washing, dry up;
(5) immerse again 0.1-5 h in the platinum acid chloride solution;
(6) repeat above-mentioned steps (4), (5), carry out layer by layer self assembly, form (polyelectrolyte/Graphene) on the conductive substrates surface m/ (polyelectrolyte/chloroplatinic acid) nThe self-assembling ultrathin film of different structure, the different numbers of plies, m, n are respectively number of repetition;
(7) with above-mentioned ultrathin membrane sintering in air, temperature is 400-600 ℃, and the time is 0.1-5 h, makes it change into (Graphene) m/ (nano platinum particle) nThe ultrathin membrane of structure.
2. preparation method according to claim 1, the material that it is characterized in that described conductive substrates is electro-conductive glass or conductive polymer membrane.
3. preparation method according to claim 1, it is characterized in that in the described polyelectrolyte solution, polyelectrolyte is diallyl dimethyl ammoniumchloride or polymine cationic polyelectrolyte, its solvent is water, absolute ethyl alcohol, ether or acetone, or several mixed solvent wherein, the mass fraction of polyelectrolyte is 0.001 %-10 %, and the pH value is 6-13.
4. described preparation method one of according to claim 1-3, the solvent that it is characterized in that described graphene suspension is water, absolute ethyl alcohol, DMF or dimethyl sulfoxide (DMSO), or several mixed solvent wherein, the mass fraction of Graphene is 0.001 %-5 %, and the pH value is 6-13.
5. preparation method according to claim 4, the solvent that it is characterized in that described platinum acid chloride solution is water, absolute ethyl alcohol, isopropyl alcohol or acetone, or several mixed solvent wherein, the mass fraction of chloroplatinic acid is 0.001 %-20 %.
CN2011101934594A 2011-07-12 2011-07-12 Method for preparing graphene/platinum nano counter electrode material for dye sensitized solar cell Expired - Fee Related CN102324319B (en)

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CN102698741B (en) * 2012-04-16 2013-11-20 中国科学院等离子体物理研究所 Method for preparing grapheme platinum nanocomposite material by using argon plasma
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CN1797793A (en) * 2004-12-27 2006-07-05 中国科学院化学研究所 Method for preparing Nano platinum carried catalysis electrode in Nano crystal sensitized solar battery
CN101474899A (en) * 2009-01-16 2009-07-08 南开大学 Grapheme-organic material layered assembling film and preparation method thereof
CN101835609A (en) * 2007-09-10 2010-09-15 三星电子株式会社 Graphene sheet and process of preparing the same

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CN1797793A (en) * 2004-12-27 2006-07-05 中国科学院化学研究所 Method for preparing Nano platinum carried catalysis electrode in Nano crystal sensitized solar battery
CN101835609A (en) * 2007-09-10 2010-09-15 三星电子株式会社 Graphene sheet and process of preparing the same
CN101474899A (en) * 2009-01-16 2009-07-08 南开大学 Grapheme-organic material layered assembling film and preparation method thereof

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