CN102709070B - For the mesoporous graphene/silicon dioxide combined counter electrode and preparation method thereof of DSSC - Google Patents
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E10/542—Dye sensitized solar cells
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Abstract
The invention discloses a kind of mesoporous graphene/silicon dioxide combined counter electrode for DSSC and preparation method thereof, this combined counter electrode is made up of conductive substrates and mesoporous graphene/silicon dioxide composite membrane, this combined counter electrode carries out according to following steps: first join in graphene oxide suspension by nano SiO 2 particle, add hydrazine hydrate solution reduction after ultrasonic disperse, after adding thermal response 1 ~ 12h at 60 ~ 110 DEG C, form the suspension of mesoporous graphene/silicon dioxide nano composite material; This hanging drop is formed mesoporous graphene/silicon dioxide film in clean conductive substrates, and the thickness repeating aforesaid operations regulation and control film is 1 ~ 20 μm, i.e. obtained described combined counter electrode.Present invention process is simple, and mild condition, prepared is high to electrode catalyst activity, cheap, greatly reduces the cost to electrode, is expected to the industrial production being applied to extensive DSSC.
Description
Technical field
The present invention relates to field of dye-sensitized solar cells, particularly a kind of mesoporous graphene/silicon dioxide combined counter electrode for DSSC and preparation method thereof.
Background technology
Current regenerative resource constantly consumes, the Pressure on Energy of facing mankind continues aggravation, research and development solar cell has apparent significance, dye-sensitized solar cells (dye-sensitized solar cells, DSSCs) be a kind of novel Photoelectrochemistry, from 1991 Lausanne, SUI senior engineer (EPFL) M.
research group (Nature since this technically makes a breakthrough of professor leader, 1991,353,737), DSSCs is with its low cost, the relatively simple feature such as manufacture craft, higher electricity conversion, obtain rapidly the extensive concern of academia and industrial quarters in the world, Europe, the United States, Deng developed country have dropped into substantial contribution research and development all.
DSSCs primarily of dye sensitization porous semi-conductor nano-crystal film, electrolyte and electrode is formed.Dye molecule excites after being subject to illumination, the conduction band of electron injection semiconductive thin film, and electronics is got back to electrode through external circuit, I
3 -ion is generating I to electrode obtaining electronics
-ion, I
-ion diffuse to semiconductive thin film restores oxidation state dyestuff, dyestuff is regenerated, I
-regeneration I after ionic reaction
3 -ion, so circulates, thus realizes opto-electronic conversion.In the process, reduce because above-mentioned reduction reaction is being very necessary to the energy ezpenditure on electrode.Therefore, as one of them important component part, there is important impact to the electricity conversion of catalytic performance on DSSCs of electrode.Because platinum has excellent conductivity, electro catalytic activity and to the electrolytical chemical stability of iodine, usually adopt platinum as catalysis material to electrode.Preparation method mainly contains magnetron sputtering (Electrochimi.Acta., 2001,46,3457) and chloroplatinic acid thermal decomposition (J.Electrochem.Soc., 1997,144,876) method such as, although have good catalysis performance and combination property, because platinum is noble metal, and preparation method consumes energy high, if these methods have obvious limitation for large-scale production.Therefore the non-platinum of development of new, cheapness and have higher catalytic activity to electrode, be one, DSSCs field study hotspot in recent years.
Wherein material with carbon element is the study hotspot in this direction always, and this is mainly because material with carbon element has good electric conductivity and electro catalytic activity, and the double stability of chemistry and heat.Graphene causes the research interest of academia in recent years, at DSSCs to also having many relevant report (ACS Nano, 2010,4,6203 in electrode; ACS Nano, 2011,5,165).But because Graphene has the feature of monoatomic layer two-dimensional structure, easily form the structure of closelypacked similar graphite, cause Graphene and electrolytical contact area limited, cannot effectively play its catalytic action.Therefore, there is porous Graphene and be expected to obtain better catalysis performance to electrode, reduction DSSCs integrated cost is had great importance.
Summary of the invention
The technical problem to be solved in the present invention be high to electrode cost for traditional platinum, consume energy the drawback such as large, provides a kind of technique simple, mild condition, cheap, mesoporous graphene/silicon dioxide combined counter electrode that catalytic activity is high and preparation method thereof.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
The present invention is used for the mesoporous graphene/silicon dioxide combined counter electrode of DSSC, it is characterized in that this combined counter electrode is formed by connecting by intermolecular force by conductive substrates (1) and mesoporous graphene/silicon dioxide composite membrane (2).Wherein said conductive substrates (1) is electro-conductive glass, conducting polymer or flexible sheet metal piece; Also be formed by connecting with intermolecular force between described mesoporous graphene/silicon dioxide composite membrane (2) intermediary hole Graphene and silicon dioxide, its thickness is 1 ~ 20 μm.
The present invention is used for the preparation method of the mesoporous graphene/silicon dioxide combined counter electrode of DSSC, carry out according to following steps: first the nano SiO 2 particle of certain size is joined in certain density graphene oxide suspension, after ultrasonic disperse, form the suspension with the graphene oxide/silica composite of certain mass ratio; Then in this suspension, add 10 ~ 100 μ L mass fractions is the hydrazine hydrate solution of 10%, after adding thermal response 1 ~ 12h at 60 ~ 110 DEG C, graphene oxide is wherein reduced to Graphene, forms the suspension of mesoporous graphene/silicon dioxide nano composite material; Finally by this hanging drop in the conductive substrates cleaned up, namely in conductive substrates, the apparent uniform mesoporous graphene/silicon dioxide film of one deck is formed after solvent evaporates is complete, the thickness repeating aforesaid operations regulation and control film is 1 ~ 20 μm, i.e. obtained described mesoporous graphene/silicon dioxide combined counter electrode.
As preferably, the particle diameter of nano SiO 2 particle of the present invention is 10 ~ 100nm; The concentration of described graphene oxide suspension is 0.1 ~ 1mg/mL; Described graphene oxide and the mass ratio of silicon dioxide are 1:0.5 ~ 5; Described solvent is water, ethanol or the mixture of the two.
After have employed technique scheme, the present invention has following beneficial effect: compare closelypacked non-porous form grapheme material, and the specific area of mesoporous graphene/silicon dioxide nano composite material improves 26 times, therefore has better electrocatalysis characteristic.Be deposited in conductive substrates by this composite material, without the need to reprocessings such as sintering, directly conduct is to application of electrode in DSSC, can obtain good energy conversion efficiency.With pure Graphene to compared with electrode, use mesoporous graphene/silicon dioxide combined counter electrode to make DSSC, energy conversion efficiency improves 68%.Present invention process is simple, mild condition, and prepared non-platinum is high to electrode catalyst activity, cheap, greatly reduce the cost to electrode, and then reduce the integrated cost of dye-sensitized solar cells, be expected to the industrial production being applied to extensive DSSC.
Accompanying drawing explanation
Fig. 1 is the structural representation of the mesoporous graphene/silicon dioxide combined counter electrode for DSSC of the present invention, and wherein (1) is conductive substrates, and (2) are mesoporous graphene/silicon dioxide composite membrane;
Fig. 2 is the pore distribution curve figure of the present invention's mesoporous graphene/silicon dioxide composite material and pure Graphene, and wherein a is the pore distribution curve figure of pure Graphene (G), b is mesoporous graphene/silicon dioxide composite material (G/SiO
2) pore distribution curve figure;
Fig. 3 is the stereoscan photograph for the preparation of the mesoporous graphene/silicon dioxide composite membrane of the mesoporous graphene/silicon dioxide combined counter electrode of DSSC in the embodiment of the present invention 1;
Fig. 4 be in the embodiment of the present invention 1 and comparative example 1,2 preparation for DSSC mesoporous graphene/silicon dioxide combined counter electrode, pure Graphene, to electrode and pyrolysis platinum, to current-voltage (I-V) curve chart of the DSSCs of electrode assembling, (effective cell area is 0.2304cm
2), wherein a is current-voltage (I-V) curve chart of pure Graphene to the DSSCs that electrode (G) is assembled, and b is mesoporous graphene/silicon dioxide combined counter electrode (G/SiO
2) current-voltage (I-V) curve chart of DSSCs assembled, c is current-voltage (I-V) curve chart of pyrolysis platinum to the DSSCs that electrode (Pt) is assembled.
Embodiment
In order to make content of the present invention more easily be clearly understood, below according to specific embodiment also by reference to the accompanying drawings, the present invention is further detailed explanation.
Embodiment 1
Be that the nano SiO 2 particle of 10nm joins in the graphene oxide water slurry of 10mL0.25mg/mL by 5mg particle diameter, after ultrasonic disperse, form the suspension that mass ratio is the graphene oxide/silica composite of 1:2; Then the mass fraction adding 25 μ L in this suspension is the hydrazine hydrate solution of 10%, after adding thermal response 2h at 100 DEG C, graphene oxide is wherein reduced to Graphene, form the suspension of mesoporous graphene/silicon dioxide nano composite material, this composite material has meso-hole structure, and specific area is 229.0m
2/ g, hole dimension is for 4nm and in comparatively narrow ditribution (as shown in Figure of description Fig. 2).Finally by this hanging drop on the electro-conductive glass cleaned up, namely on electro-conductive glass, the apparent uniform mesoporous graphene/silicon dioxide film of one deck is formed after moisture evaporation is complete, the thickness repeating aforesaid operations regulation and control film is 2.5 μm, i.e. obtained described mesoporous graphene/silicon dioxide combined counter electrode.Then using this electrode as to application of electrode in DSSC.
According to standard method, this is become DSSCs to electrode assembling, wherein dyestuff adopts N719, electrolyte 0.1M LiI/0.05M I
2/ 0.5M is to the acetonitrile solution of tert .-butylpyridine/0.6M iodo 1,2-dimethyl-3-n-pro-pyl imidazoles, and cell area is 0.2304cm
2.At AM1.5 simulated solar irradiation (100mW/cm
2) under record current-voltage (I-V) curve (as shown in Figure of description Fig. 4) of DSSC, obtaining open-circuit photovoltage (Voc) is 719mV, and short-circuit photocurrent (Jsc) is 15.52mA/cm
2, fill factor, curve factor (FF) is 0.61, and energy conversion efficiency (η) is 6.81%.
Embodiment 2
Be that the nano SiO 2 particle of 50nm joins in the graphene oxide water slurry of 10mL0.1mg/mL by 0.5mg particle diameter, after ultrasonic disperse, form the suspension that mass ratio is the graphene oxide/silica composite of 1:0.5; Then the mass fraction adding 10 μ L in this suspension is the hydrazine hydrate solution of 10%, after adding thermal response 1h, graphene oxide is wherein reduced to Graphene at 110 DEG C, forms the suspension of mesoporous graphene/silicon dioxide nano composite material; Finally by this hanging drop on the electro-conductive glass cleaned up, namely on electro-conductive glass, the apparent uniform mesoporous graphene/silicon dioxide film of one deck is formed after moisture evaporation is complete, the thickness repeating aforesaid operations regulation and control film is 1 μm, i.e. obtained described mesoporous graphene/silicon dioxide combined counter electrode.Then using this electrode as to application of electrode in DSSC.
According to standard method, this is become DSSCs to electrode assembling, wherein dyestuff adopts N719, electrolyte 0.1M LiI/0.05M I
2/ 0.5M is to the acetonitrile solution of tert .-butylpyridine/0.6M iodo 1,2-dimethyl-3-n-pro-pyl imidazoles, and cell area is 0.2304cm
2.At AM1.5 simulated solar irradiation (100mW/cm
2) under record the I-V curve of DSSC, to obtain Voc be 704mV, Jsc be 15.84mA/cm2, FF be 0.43, η is 4.78%.
Embodiment 3
Be that the nano SiO 2 particle of 100nm joins in the graphene oxide water slurry of 10mL1mg/mL by 50mg particle diameter, after ultrasonic disperse, form the suspension that mass ratio is the graphene oxide/silica composite of 1:5; Then the mass fraction adding 100 μ L in this suspension is the hydrazine hydrate solution of 10%, after adding thermal response 12h, graphene oxide is wherein reduced to Graphene at 60 DEG C, forms the suspension of mesoporous graphene/silicon dioxide nano composite material; Finally by this hanging drop on the electro-conductive glass cleaned up, namely on electro-conductive glass, the apparent uniform mesoporous graphene/silicon dioxide film of one deck is formed after moisture evaporation is complete, the thickness repeating aforesaid operations regulation and control film is 20 μm, i.e. obtained described mesoporous graphene/silicon dioxide combined counter electrode.Then using this electrode as to application of electrode in DSSC.
According to standard method, this is become DSSCs to electrode assembling, wherein dyestuff adopts N719, electrolyte 0.1M LiI/0.05M I
2/ 0.5M is to the acetonitrile solution of tert .-butylpyridine/0.6M iodo 1,2-dimethyl-3-n-pro-pyl imidazoles, and cell area is 0.2304cm
2.At AM1.5 simulated solar irradiation (100mW/cm
2) under record the I-V curve of DSSC, to obtain Voc be 683mV, Jsc is 11.14mA/cm
2, FF is 0.52, η is 3.96%.
Embodiment 4
Be that the nano SiO 2 particle of 10nm joins in the graphene oxide alcohol suspension of 10mL0.1mg/mL by 1mg particle diameter, after ultrasonic disperse, form the suspension that mass ratio is the graphene oxide/silica composite of 1:1; Then the mass fraction adding 10 μ L in this suspension is the hydrazine hydrate solution of 10%, after adding thermal response 6h, graphene oxide is wherein reduced to Graphene at 80 DEG C, forms the suspension of mesoporous graphene/silicon dioxide nano composite material; Finally by this hanging drop on the PET conductive plastics cleaned up, namely on electro-conductive glass, the apparent uniform mesoporous graphene/silicon dioxide film of one deck is formed after ethanol volatilization completely, the thickness repeating aforesaid operations regulation and control film is 2 μm, i.e. obtained described mesoporous graphene/silicon dioxide combined counter electrode.Then using this electrode as to application of electrode in DSSC.
According to standard method, this is become DSSCs to electrode assembling, wherein dyestuff adopts N719, electrolyte 0.1M LiI/0.05M I
2/ 0.5M is to the acetonitrile solution of tert .-butylpyridine/0.6M iodo 1,2-dimethyl-3-n-pro-pyl imidazoles, and cell area is 0.2304cm
2.At AM1.5 simulated solar irradiation (100mW/cm
2) under record the I-V curve of DSSC, to obtain Voc be 706mV, Jsc is 12.29mA/cm
2, FF is 0.42, η is 3.64%.
Embodiment 5
Be that the nano SiO 2 particle of 10nm joins in graphene oxide water/ethanol (volume ratio 1:1) suspension of 10mL0.2mg/mL by 6mg particle diameter, after ultrasonic disperse, form the suspension that mass ratio is the graphene oxide/silica composite of 1:3; Then the mass fraction adding 20 μ L in this suspension is the hydrazine hydrate solution of 10%, after adding thermal response 12h, graphene oxide is wherein reduced to Graphene at 60 DEG C, forms the suspension of mesoporous graphene/silicon dioxide nano composite material; Finally by this hanging drop in the titanium sheet cleaned up (thickness is about 0.1mm), namely on electro-conductive glass, the apparent uniform mesoporous graphene/silicon dioxide film of one deck is formed after solvent evaporates to be mixed is complete, the thickness repeating aforesaid operations regulation and control film is 3 μm, i.e. obtained described mesoporous graphene/silicon dioxide combined counter electrode.Then using this electrode as to application of electrode in DSSC.
According to standard method, this is become DSSCs to electrode assembling, wherein dyestuff adopts N719, electrolyte 0.1M LiI/0.05M I
2/ 0.5M is to the acetonitrile solution of tert .-butylpyridine/0.6M iodo 1,2-dimethyl-3-n-pro-pyl imidazoles, and cell area is 0.2304cm
2.At AM1.5 simulated solar irradiation (100mW/cm
2) under record the I-V curve of DSSC, to obtain Voc be 701mV, Jsc is 13.55mA/cm
2, FF is 0.41, η is 3.89%.
Embodiment 6
Be that the nano SiO 2 particle of 10nm joins in the graphene oxide water slurry of 10mL0.25mg/mL by 5mg particle diameter, after ultrasonic disperse, form the suspension that mass ratio is the graphene oxide/silica composite of 1:2; Then the mass fraction adding 25 μ L in this suspension is the hydrazine hydrate solution of 10%, after adding thermal response 2h, graphene oxide is wherein reduced to Graphene at 100 DEG C, forms the suspension of mesoporous graphene/silicon dioxide nano composite material; Finally by this hanging drop on the stainless steel substrates cleaned up (thickness is about 0.1mm), namely on electro-conductive glass, the apparent uniform mesoporous graphene/silicon dioxide film of one deck is formed after moisture evaporation is complete, the thickness repeating aforesaid operations regulation and control film is 2 μm, i.e. obtained described mesoporous graphene/silicon dioxide combined counter electrode.Then using this electrode as to application of electrode in DSSC.
According to standard method, this is become DSSCs to electrode assembling, wherein dyestuff adopts N719, electrolyte 0.1M LiI/0.05M I
2/ 0.5M is to the acetonitrile solution of tert .-butylpyridine/0.6M iodo 1,2-dimethyl-3-n-pro-pyl imidazoles, and cell area is 0.2304cm
2.At AM1.5 simulated solar irradiation (100mW/cm
2) under record the I-V curve of DSSC, to obtain Voc be 698mV, Jsc is 13.12mA/cm
2, FF is 0.42, η is 3.85%.
Comparing embodiment 1
As a comparison, we have prepared pure Graphene in the same way to electrode, its specific area has been 8.6m
2/ g, is non-pore structure (shown in Figure of description Fig. 2).Assemble DSSCs when every other condition is identical, wherein dyestuff adopts N719, electrolyte 0.1M LiI/0.05M I
2/ 0.5M is to the acetonitrile solution of tert .-butylpyridine/0.6M iodo 1,2-dimethyl-3-n-pro-pyl imidazoles.At AM 1.5 simulated solar irradiation (100mW/cm
2) under record the I-V curve (Figure of description Fig. 4) of DSSC, to obtain Voc be 723mV, Jsc is 15.17mA/cm
2, FF is 0.37, η is 4.06%.
Comparing embodiment 2
As a comparison, we are also when every other condition is identical, the DSSC that adopted pyrolysis platinum to electrode assembling, wherein dyestuff adopts N719, electrolyte 0.1M LiI/0.05M I
2/ 0.5M is to the acetonitrile solution of tert .-butylpyridine/0.6M iodo 1,2-dimethyl-3-n-pro-pyl imidazoles.At AM 1.5 simulated solar irradiation (100mW/cm
2) under record the I-V curve (Figure of description Fig. 4) of DSSC, to obtain Voc be 724mV, Jsc is 15.79mA/cm
2, FF is 0.64, η is 7.32%.
According to mesoporous graphene/silicon dioxide combined counter electrode prepared by the embodiment of the present invention 1, energy conversion efficiency exceedes pure Graphene to electrode 67%, reaches the level suitable to electrode with pyrolysis platinum.Present invention process is simple, and raw graphite, nano SiO 2 particle are cheap material, thus greatly reduce the manufacturing cost to electrode and even DSSCs, are expected to the large-scale production being applied to DSSCs.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; be understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. the preparation method for the mesoporous graphene/silicon dioxide combined counter electrode of DSSC, it is characterized in that the method is carried out according to following steps: first join in certain density graphene oxide suspension by the nano SiO 2 particle of certain size, after ultrasonic disperse, form the suspension with the graphene oxide/silica composite of certain mass ratio; Then in this suspension, add 10 ~ 100 μ L mass fractions is the hydrazine hydrate solution of 10%, after adding thermal response 1 ~ 12h at 60 ~ 110 DEG C, graphene oxide is wherein reduced to Graphene, forms the suspension of mesoporous graphene/silicon dioxide nano composite material; Finally by this hanging drop in the conductive substrates cleaned up, namely in conductive substrates, the apparent uniform mesoporous graphene/silicon dioxide film of one deck is formed after solvent evaporates is complete, the thickness repeating aforesaid operations regulation and control film is 1 ~ 20 μm, i.e. obtained described mesoporous graphene/silicon dioxide combined counter electrode.
2. the preparation method of a kind of mesoporous graphene/silicon dioxide combined counter electrode for DSSC according to claim 1, is characterized in that the particle diameter of described nano SiO 2 particle is 10 ~ 100nm.
3. the preparation method of a kind of mesoporous graphene/silicon dioxide combined counter electrode for DSSC according to claim 1, is characterized in that the concentration of described graphene oxide suspension is 0.1 ~ 1mg/mL.
4. the preparation method of a kind of mesoporous graphene/silicon dioxide combined counter electrode for DSSC according to claim 1, is characterized in that the mass ratio of described graphene oxide and silicon dioxide is 1:0.5 ~ 5.
5. the preparation method of a kind of mesoporous graphene/silicon dioxide combined counter electrode for DSSC according to claim 1, is characterized in that described solvent is water, ethanol or the mixture of the two.
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Granted publication date: 20150729 Termination date: 20200725 |
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| CF01 | Termination of patent right due to non-payment of annual fee |