CN102543256A - Chloroplatinic acid slurry, preparation method thereof, counter electrode, and dye-sensitized solar cell - Google Patents
Chloroplatinic acid slurry, preparation method thereof, counter electrode, and dye-sensitized solar cell Download PDFInfo
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- CN102543256A CN102543256A CN2012100678260A CN201210067826A CN102543256A CN 102543256 A CN102543256 A CN 102543256A CN 2012100678260 A CN2012100678260 A CN 2012100678260A CN 201210067826 A CN201210067826 A CN 201210067826A CN 102543256 A CN102543256 A CN 102543256A
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- 239000002253 acid Substances 0.000 title claims abstract description 86
- 239000002002 slurry Substances 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 46
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 26
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 26
- RBNWAMSGVWEHFP-UHFFFAOYSA-N trans-p-Menthane-1,8-diol Chemical compound CC(C)(O)C1CCC(C)(O)CC1 RBNWAMSGVWEHFP-UHFFFAOYSA-N 0.000 claims description 18
- 206010070834 Sensitisation Diseases 0.000 claims description 6
- 230000008313 sensitization Effects 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 abstract description 87
- 229910052697 platinum Inorganic materials 0.000 abstract description 44
- 238000000034 method Methods 0.000 abstract description 13
- 238000006243 chemical reaction Methods 0.000 abstract description 12
- 230000005540 biological transmission Effects 0.000 abstract description 4
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 abstract 2
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 abstract 2
- 229940116411 terpineol Drugs 0.000 abstract 2
- 239000003792 electrolyte Substances 0.000 description 9
- 238000003756 stirring Methods 0.000 description 8
- 238000001548 drop coating Methods 0.000 description 7
- 239000011521 glass Substances 0.000 description 7
- 238000007639 printing Methods 0.000 description 7
- 238000007650 screen-printing Methods 0.000 description 7
- 238000011160 research Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 4
- 229910052724 xenon Inorganic materials 0.000 description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000007613 slurry method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000001235 sensitizing effect Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 150000003057 platinum Chemical class 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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Abstract
The invention discloses chloroplatinic acid slurry, a preparation method thereof, a counter electrode of a dye-sensitized solar cell prepared from the slurry, and the dye-sensitized solar cell. The slurry consists of chloroplatinic acid, isopropyl alcohol, terpineol and polyethylene glycol. In the preparation process of the slurry, the terpineol and the polyethylene glycol are mixed so as to obtain an organic carrier of a chloroplatinic-acid-containing isopropyl alcohol solution. The chloroplatinic acid slurry which is prepared by the method is uniform in thickness on the surface of a platinum counter electrode and is high in uniformity, so that the transmission speed of electrons on the counter electrode and the photocatalytic effect are improved, and the photoelectric conversion rate of the dye-sensitized solar cell is improved.
Description
Technical field
The present invention relates to a kind of field of dye-sensitized solar cells, the DSSC that is specifically related to a kind of chloroplatinic acid slurry and preparation method thereof and this pulp preparation of use is to electrode and DSSC.
Background technology
Professors Greatzel of engineering institute such as Lausanne, SUI height leader's in 1991 research group is nanoporous TiO
2Be applied to DSSC, this research has obtained breakthrough.Teach in the laboratory small size (＜0.2cm from Gratzel
2) battery obtained since 7.1% the photoelectric conversion efficiency, DSSC has caused that increasing scientist payes attention to, and brings up to 11.04% small size battery efficiency in 2004, present Japanese Sharp company announces that the small size battery reaches 11.1%.Because the potential application prospect of DSSC (DSSC) has attracted numerous commercial companies and research institution to drop into a large amount of strength, and the research that has strengthened the area battery with practicability meaning.
DSSC is mainly formed by light anode, nano porous semiconductor film, dye sensitizing agent, electrolyte with to several parts of electrode.This battery is with I
3 -/ I
-Oxidation-reduction pair is that media transmits electric charge at the light anode with between to electrode, in the circulation of this media regeneration, and oxidized material (I
2Or I
3 -) on to electrode, be reduced to I again
-Therefore, be the important component part of DSSC to electrode, electrode there are two important function in battery: the one, collect the electronics that transmits from the light anode, the 2nd, catalysis I
3 -Ion plays transmission electronic and light-catalysed effect in the reduction reaction of light anode to electrode, to electrode the charge migration on the electrolyte interface is rapidly and efficiently carried out, and has reduced the electron recombination probability, has suppressed dark current, has improved the photoelectric conversion efficiency of battery.
At present, to electrode according to materials used different divide platinum to electrode and carbon to electrode.Carbon to the adhesion of electrode and substrate of glass a little less than, cause the photoelectric properties of battery and long-time stability all relatively poor, therefore, platinum becomes the focus of research to electrode.Carrying platinum mainly contains the preparation method of electrode: pyrolysismethod, magnetron sputtering and electrodeposition process etc.Wherein the prepared electrode platinum content of magnetron sputtering and electro-deposition is higher, causes cost to increase, and pyrolysismethod has exactly been avoided this kind defective and become the focus of research.Pyrolysismethod platinum adopts drop-coating to electrode preparation more; The subject matter of drop-coating is that the viscosity of platinum acid chloride solution is little, and the thickness of wayward rete and uniformity during coating cause platinum layer variable thickness, the lack of homogeneity of preparation; The face resistance of platinum layer is inhomogeneous; Thereby influence electric transmission speed and photocatalysis effect, influence photoelectric conversion efficiency, and repeatability is relatively poor.
Summary of the invention
Technical problem to be solved by this invention is to the above-mentioned deficiency that exists in the prior art, and the DSSC that a kind of chloroplatinic acid slurry and preparation method thereof and this pulp preparation of use are provided is to electrode and DSSC.This preparation technology is simple, and to electrode platinum layer thickness uniformity, good reproducibility, low to the DSSC cost that electrode makes by this platinum, photoelectric conversion efficiency is high by the platinum of the platinum pulp preparation of this preparation method preparation.
Solving the technical scheme that technical problem of the present invention adopted is a kind of chloroplatinic acid slurry, is made up of following material: chloroplatinic acid, isopropyl alcohol, terpinol and polyethylene glycol.
Preferably, the molecular weight of polyethylene glycol is 2000～20000 in the said chloroplatinic acid slurry.
More preferably, the molecular weight of polyethylene glycol is 8000～20000 in the said chloroplatinic acid slurry.
Preferably, the preparation process of said chloroplatinic acid slurry comprises: the aqueous isopropanol of the chloroplatinic acid of preparation 1mmol/L～20mmol/L; Is the mixed of (1: 8)～(3: 1) with polyethylene glycol and terpinol according to mass ratio, obtains organic carrier; Is the mixed of (2: 1)～(5: 1) with the aqueous isopropanol and the organic carrier of chloroplatinic acid according to volume ratio, obtains the chloroplatinic acid slurry.
More preferably, above-mentioned polyethylene glycol and terpinol are the mixed of (1: 5)～(1: 3) according to mass ratio.
Preferably, the viscosity of said organic carrier is 2～6Pa.s, and the viscosity of chloroplatinic acid slurry is 1～5Pa.s.
The present invention also provides a kind of preparation method of chloroplatinic acid slurry, may further comprise the steps:
(1) aqueous isopropanol of preparation chloroplatinic acid; Polyethylene glycol is mixed with terpinol, obtain organic carrier;
(2) aqueous isopropanol with chloroplatinic acid mixes with organic carrier, obtains the chloroplatinic acid slurry.
Preferably, the concentration of the aqueous isopropanol of the chloroplatinic acid of preparation is 1 mmol/L～20mmol/L in the said step (1).
Preferably, the molecular weight of polyethylene glycol is 2000～20000 in the said step (1), and the mass ratio of polyethylene glycol and terpinol is (1: 8)～(3: 1), and the viscosity of the organic carrier that obtains is 2～6Pa.s.
More preferably, the molecular weight of polyethylene glycol is 8000～20000 in the said step (1), and the mass ratio of polyethylene glycol and terpinol is (1: 5)～(1: 3), and the viscosity of the organic carrier that obtains is 4～6Pa.s.
Preferably, the polyethylene glycol in the step (1) mixes under 30～70 ℃ with terpinol, stirs 0.5～5 hour.
More preferably, the polyethylene glycol in the step (1) mixes under 30～60 ℃ with terpinol, stirs 1～3.5 hour.
Preferably, the aqueous isopropanol of the chloroplatinic acid in the said step (2) and the volume ratio of organic carrier are (2: 1)～(5: 1), and the viscosity of the chloroplatinic acid slurry that obtains is 1～5Pa.s.
The present invention also provide a kind of used by dye sensitization solar battery to electrode, it is for using above-mentioned chloroplatinic acid pulp preparation.
The present invention also provides a kind of DSSC, it comprise above-mentioned used by dye sensitization solar battery to electrode.
Description of drawings
Fig. 1 is that the platinum of traditional drop-coating preparation is to the electrode surface shape appearance figure;
Fig. 2 is that the platinum of method preparation of the embodiment of the invention 1 is to the electrode surface shape appearance figure;
Fig. 3 is that the platinum of traditional drop-coating preparation is to the pairing cell I-V detection of electrode figure;
Fig. 4 is that the platinum of the embodiment of the invention 1 preparation is to the pairing cell I-V detection of electrode figure.
Embodiment
For making those skilled in the art understand technical scheme of the present invention better, the present invention is described in further detail below in conjunction with accompanying drawing and embodiment.
Embodiment 1
The aqueous isopropanol of the chloroplatinic acid of preparation 10mmol/L; Be that 6000 polyethylene glycol mixes with terpinol with molecular weight, both mass ratioes are 3: 1, stir down at 45 ℃ and obtain organic carrier in 1 hour, and the viscosity of organic carrier is 3Pa.s; The aqueous isopropanol of chloroplatinic acid is mixed with organic carrier, and both volume ratios are 3: 1, obtain the chloroplatinic acid slurry, and the viscosity of chloroplatinic acid slurry is 1.8Pa.s.
The method of the chloroplatinic acid slurry for preparing with silk screen printing evenly is printed on the clean conductive glass, and it is 200 orders that half tone order number is used in printing.With apply slurry to electrode in 80 ℃ of dry 30min, 30min is fired in the back under 450 ℃, make chloroplatinic acid resolve into platinum, promptly makes platinum to electrode.Platinum is docked with the light anode electrode, splash into electrolyte, be assembled into DSSC, its efficient of test under xenon lamp simulated solar light source.Survey efficient institute use xenon lamp simulated solar irradiation, light intensity is 100mW/cm
2(measuring light intensity with the standard silicon photodiode) under this light intensity, records the cell photoelectric conversion efficiency that this membrane electrode is formed.
The viscosity of the chloroplatinic acid slurry of conventional method preparation is low, can only use drop-coating that platinum is applied electrode.As shown in Figure 1, the platinum of traditional drop-coating preparation is inhomogeneous to the electrode surface pattern, and a lot of cracks are arranged.The chloroplatinic acid slurry of the present invention's preparation can adopt several different methods that platinum is applied electrode owing to have certain viscosity.As shown in Figure 2, use method for printing screen that platinum is applied electrode, the platinum that obtains is smooth evenly to the electrode surface pattern; Platinum layer has uniformity consistency, makes face resistance become evenly, thereby has improved electric transmission speed and photocatalysis effect; Improved the photoelectric conversion efficiency of DSSC; And good reproducibility, and use screen printing technique to prepare platinum to electrode, can prepare uniform large-area platinum to electrode.
The platinum of tradition drop-coating preparation is as shown in Figure 3 to the I-V detection figure of the DSSC that electrode pair is answered, and can find out that from test result the short-circuit current density of battery is 7.38mA/cm
2, open circuit voltage is 0.765V, and fill factor, curve factor is 64.94%, and photoelectric conversion efficiency is 3.67%.It is as shown in Figure 4 that the I-V of the DSSC of the present invention's preparation detects figure, and the short-circuit current density of battery is 1 0.4mA/cm
2, open circuit voltage is 0.759V, and fill factor, curve factor is 62.32%, and photoelectric conversion efficiency is 4.92%, and the photoelectric conversion rate of the DSSC of the present invention's preparation improves compared with conventional method.
Embodiment 2
The aqueous isopropanol of the chloroplatinic acid of preparation 5mmol/L; Be that 4000 polyethylene glycol mixes with terpinol with molecular weight, both mass ratioes are 1: 4, stir down at 30 ℃ and obtain organic carrier in 5 hours, and the viscosity of organic carrier is 2.5Pa.s; The aqueous isopropanol of chloroplatinic acid is mixed with organic carrier, and both volume ratios are 2: 1, obtain the chloroplatinic acid slurry, and the viscosity of chloroplatinic acid slurry is 1.5Pa.s.
The method of the chloroplatinic acid slurry for preparing with silk screen printing evenly is printed on the clean conductive glass, and it is 200 orders that half tone order number is used in printing.With apply slurry to electrode in 80 ℃ of dry 30min, 30min is fired in the back under 450 ℃, make chloroplatinic acid resolve into platinum, promptly makes platinum to electrode.Platinum is docked with the light anode electrode, splash into electrolyte, be assembled into DSSC, its efficient of test under xenon lamp simulated solar light source.Survey efficient institute use xenon lamp simulated solar irradiation, light intensity is 1 00mW/cm
2(measuring light intensity with the standard silicon photodiode) under this light intensity, records the cell photoelectric conversion efficiency that this membrane electrode is formed.
It is as shown in Figure 2 that the I-V of the DSSC that present embodiment is corresponding detects figure, can find out that from test result the short-circuit current density of battery is 1 0.4mA/cm
2, open circuit voltage is 0.759V, and fill factor, curve factor is 62.32%, and photoelectric conversion efficiency is 4.92%.
Embodiment 3
The aqueous isopropanol of the chloroplatinic acid of preparation 20mmol/L; Be that 20000 polyethylene glycol mixes with terpinol with molecular weight, both mass ratioes are 1: 3, stir down at 55 ℃ and obtain organic carrier in 0.5 hour, and the viscosity of organic carrier is 6Pa.s; The aqueous isopropanol of chloroplatinic acid is mixed with organic carrier, and both volume ratios are 5: 2, obtain the chloroplatinic acid slurry, and the viscosity of chloroplatinic acid slurry is 5Pa.s.
The method of the chloroplatinic acid slurry for preparing with silk screen printing evenly is printed on the clean conductive glass, and it is 200 orders that half tone order number is used in printing.With apply slurry to electrode in 80 ℃ of dry 30min, 30min is fired in the back under 450 ℃, make chloroplatinic acid resolve into platinum, promptly makes platinum to electrode.Platinum is docked with the light anode electrode, splash into electrolyte, be assembled into DSSC.
Embodiment 4
The aqueous isopropanol of the chloroplatinic acid of preparation 1mmol/L; Be that 2000 polyethylene glycol mixes with terpinol with molecular weight, both mass ratioes are 1: 8, stir down at 50 ℃ and obtain organic carrier in 2.2 hours, and the viscosity of organic carrier is 2Pa.s; The aqueous isopropanol of chloroplatinic acid is mixed with organic carrier, and both volume ratios are 4: 1, obtain the chloroplatinic acid slurry, and the viscosity of chloroplatinic acid slurry is 1Pa.s.
The method of the chloroplatinic acid slurry for preparing with silk screen printing evenly is printed on the clean conductive glass, and it is 200 orders that half tone order number is used in printing.With apply slurry to electrode in 80 ℃ of dry 30min, 30min is fired in the back under 450 ℃, make chloroplatinic acid resolve into platinum, promptly makes platinum to electrode.Platinum is docked with the light anode electrode, splash into electrolyte, be assembled into DSSC.
Embodiment 5
The aqueous isopropanol of the chloroplatinic acid of preparation 15mmol/L; Be that 8000 polyethylene glycol mixes with terpinol with molecular weight, both mass ratioes are 2: 1, stir down at 60 ℃ and obtain organic carrier in 3.5 hours, and the viscosity of organic carrier is 4Pa.s; The aqueous isopropanol of chloroplatinic acid is mixed with organic carrier, and both volume ratios are 5: 1, obtain the chloroplatinic acid slurry, and the viscosity of chloroplatinic acid slurry is 2Pa.s.
The method of the chloroplatinic acid slurry for preparing with silk screen printing evenly is printed on the clean conductive glass, and it is 200 orders that half tone order number is used in printing.With apply slurry to electrode in 80 ℃ of dry 30min, 30min is fired in the back under 450 ℃, make chloroplatinic acid resolve into platinum, promptly makes platinum to electrode.Platinum is docked with the light anode electrode, splash into electrolyte, be assembled into DSSC.
Embodiment 6
The aqueous isopropanol of the chloroplatinic acid of preparation 12mmol/L; Be that 10000 polyethylene glycol mixes with terpinol with molecular weight, both mass ratioes are 1: 5, stir down at 70 ℃ and obtain organic carrier in 3.2 hours, and the viscosity of organic carrier is 5Pa.s; The aqueous isopropanol of chloroplatinic acid is mixed with organic carrier, and both volume ratios are 7: 2, obtain the chloroplatinic acid slurry, and the viscosity of chloroplatinic acid slurry is 3Pa.s.
The method of the chloroplatinic acid slurry for preparing with silk screen printing evenly is printed on the clean conductive glass, and it is 200 orders that half tone order number is used in printing.With apply slurry to electrode in 80 ℃ of dry 30min, 30min is fired in the back under 450 ℃, make chloroplatinic acid resolve into platinum, promptly makes platinum to electrode.Platinum is docked with the light anode electrode, splash into electrolyte, be assembled into DSSC.
Embodiment 7
Present embodiment provides a kind of chloroplatinic acid slurry, and it is by method for preparing.
Embodiment 8
Present embodiment provide a kind of used by dye sensitization solar battery to electrode, it uses above-mentioned chloroplatinic acid slurry to make.
Embodiment 9
Present embodiment provides a kind of DSSC, its use above-mentioned used by dye sensitization solar battery to electrode.
Certainly, the DSSC of this enforcement also comprises other material known such as light anode, nano porous semiconductor film, dye sensitizing agent, electrolyte, element etc.
It is understandable that above execution mode only is the illustrative embodiments that adopts for principle of the present invention is described, yet the present invention is not limited thereto.For the one of ordinary skilled in the art, under the situation that does not break away from spirit of the present invention and essence, can make various modification and improvement, these modification also are regarded as protection scope of the present invention with improving.
Claims (10)
1. a chloroplatinic acid slurry is characterized in that, is made up of following material: chloroplatinic acid, isopropyl alcohol, terpinol and polyethylene glycol.
2. chloroplatinic acid slurry according to claim 1 is characterized in that, the molecular weight of said polyethylene glycol is 2000～20000.
3. chloroplatinic acid slurry according to claim 1 is characterized in that, the preparation process of said chloroplatinic acid slurry comprises: the aqueous isopropanol of the chloroplatinic acid of preparation 1mmol/L～20mmol/L; Is the mixed of (1: 8)～(3: 1) with polyethylene glycol and terpinol according to mass ratio, obtains organic carrier; Is the mixed of (2: 1)～(5: 1) with the aqueous isopropanol and the organic carrier of chloroplatinic acid according to volume ratio, obtains the chloroplatinic acid slurry.
4. chloroplatinic acid slurry according to claim 3 is characterized in that, the viscosity of said organic carrier is 2～6Pa.s, and the viscosity of chloroplatinic acid slurry is 1～5Pa.s.
5. the preparation method of a chloroplatinic acid slurry is characterized in that, may further comprise the steps:
(1) aqueous isopropanol of preparation chloroplatinic acid; Polyethylene glycol is mixed with terpinol, obtain organic carrier;
(2) aqueous isopropanol with chloroplatinic acid mixes with organic carrier, obtains the chloroplatinic acid slurry.
6. the preparation method of chloroplatinic acid slurry according to claim 5 is characterized in that, the concentration of the aqueous isopropanol of the chloroplatinic acid of preparation is 1mmol/L～20mmol/L in the said step (1).
7. the preparation method of chloroplatinic acid slurry according to claim 5; It is characterized in that; The molecular weight of polyethylene glycol is 2000～20000 in the said step (1), and the mass ratio of polyethylene glycol and terpinol is (1: 8)～(3: 1), and the viscosity of the organic carrier that obtains is 2～6Pa.s.
8. the preparation method of chloroplatinic acid slurry according to claim 5 is characterized in that, the aqueous isopropanol of the chloroplatinic acid in the said step (2) and the volume ratio of organic carrier are (2: 1)～(5: 1), and the viscosity of the chloroplatinic acid slurry that obtains is 1～5Pa.s.
A used by dye sensitization solar battery to electrode, it is characterized in that it is to use any described chloroplatinic acid pulp preparation in the claim 1 to 4.
10. a DSSC is characterized in that, it comprise the described used by dye sensitization solar battery of claim 9 to electrode.
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