CN105304338A - Counter electrode for quantum-dot sensitized solar cell and manufacturing method thereof - Google Patents
Counter electrode for quantum-dot sensitized solar cell and manufacturing method thereof Download PDFInfo
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- CN105304338A CN105304338A CN201510252312.6A CN201510252312A CN105304338A CN 105304338 A CN105304338 A CN 105304338A CN 201510252312 A CN201510252312 A CN 201510252312A CN 105304338 A CN105304338 A CN 105304338A
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Abstract
The invention discloses a counter electrode for a quantum-dot sensitized solar cell and a manufacturing method thereof. According to the counting scheme of the invention, the structure of the counter electrode is that a catalyst layer formed by PbS and CuS grows on the surface of an FTO conductive glass substrate, and the catalyst layer is manufactured by adopting a low-temperature chemical bath deposition method. the problems that the existing Pt counter electrode is high in cost and low in catalytic performance and a metal sulfide counter electrode is poor in stability and not easy to package are solved, and the counter electrode manufactured in the invention is low in cost, high in catalytic activities and simple in manufacturing process.
Description
technical field:
The invention belongs to field of solar energy utilization, also belong to field of nanometer material technology, be specifically related to a kind of Pb for quantum dot sensitized solar cell
xcu
1-xs is to electrode and preparation method thereof
background technology:
The Heavy environmental pollution brought in the day by day exhausted of fossil energy and use procedure thereof, inexhaustible solar energy becomes the important countermeasure addressed this problem.In all kinds of novel solar battery, preparation technology's quantum dot sensitized solar cell (QDSSC) simple, with low cost causes the extensive concern of researcher.Compared with dye sensitizing agent, quantum dot has adjustable band structure, higher extinction coefficient, the advantage (A.Kongkanand, etal., J.Am.Chem.Soc., 2008,130,4007) that larger natural dipole moment and exciton multiplier effect etc. are unique.Therefore, study QDSSC to have very important significance to developing low-cost, high efficiency solar cell.
QDSSC, primarily of the absorption light anode of quantum dot, electrolyte and to electrode three part composition, is wherein that the electron transmission of external circuit is made its reducing/regenerating to electrolyte to the effect of electrode.In addition, the electron exchange speed in electrolyte between redox couple and negative electrode can also be accelerated to electrode, play catalytic action.I
-/ I
3 -be electrolyte conventional in DSSC, precious metals pt is to I
-/ I
3 -there is high catalytic activity and chemical stability, to the Charge-transfer resistance (R at electrode/electrolyte interface
ct) very low, thus Pt is the most frequently used to electrode in dye-sensitized cell.But most of quanta point material is at I
-/ I
3 -can be unstable due to chemical corrosion in electrolyte, thus conventional many sulphur electrolyte (S in the research of QDSSC
2-/ S
n 2-) replace I
-/ I
3 -as the hole-conductive layer of battery.But at S
2-/ S
n 2-in system, the catalytic activity of the noble metal electrodes such as Pt is very low, causes the Charge-transfer resistance at electrode/electrolyte interface very large, and this causes the fill factor, curve factor of QDSSC and a photoelectric conversion efficiency major reason on the low side.In addition, the S in many sulphur electrolyte
2-be easy to be adsorbed onto Pt surface, produce poison effect, affect the stability (J.G.Radich, etal., J.Phys.Chem.Lett., 2011,2,2453) to electrode, so, Pt be not be applicable to QDSSC optimum to electrode material.In order to reduce the Charge-transfer resistance to electrode/electrolyte interface, multiple material attempted as to application of electrode in QDSSC, such as Cu
2s(Pan.Z, etal., ACSNano, 2013,7 (6): 5215), PbS(Tachan.Z, etal., J.Phys.Chem.C, 2011,115 (13): 6162), CoS(Yuan.H, etal., J.Electrochem.Soc., 2013,160 (9): H624) etc., this several metal sulfide has higher catalytic activity to electrode material compared with Pt, and cost is also lower, but this several preparation method to electrode normally first adopts HCl or H at present
2sO4 corroding metal (Cu, Pb etc.) paillon foil, then many sulphur electrolyte is dropped in foil surfaces, thus form layer of metal sulfide (Tachan.Z at metal foil surface, etal., J.Phys.Chem.C, 2011,115 (13): 6162, G.Hodes, etal., J.Electrochem.Soc., 127 (3): 544), although this preparation method is easier, can corroding metal paillon foil constantly owing to be packaged into after battery electrolyte, very poor to the stability of electrode; And because this several metal sulfide is all corrode to form on tinsel to electrode, between metal sulfide and foil substrate, adhesiveness is very poor, add metal foil surface more coarse, there is the problem being difficult to encapsulate, be therefore difficult to meet practical needs.
summary of the invention:
Problem to be solved by this invention be high to electrode cost for existing Pt, catalytic performance is low and metal sulfide is poor to electrode stability, the problem that not easily encapsulates, provide a kind of with low cost, catalytic activity is higher, preparation technology is simple, can the Pb for QDSSC for preparing of large area
xcu
1-xs is to electrode and preparation method thereof.This to electrode by low temperature solution polycondensation FTO electro-conductive glass substrate surface deposition form, combining closely between electrode material and substrate of formation, and Pb
xcu
1-xs thickness is controlled, is easy to encapsulation, can significantly improves the photoelectric conversion efficiency of QDSSC.
For achieving the above object, the technical solution used in the present invention is:
A kind of for quantum dot sensitized solar cell to electrode and preparation method thereof, it is characterized in that: be grow at FTO electro-conductive glass substrate surface the Catalytic Layer that one deck is made up of PbS and CuS to the structure of electrode, this Catalytic Layer adopts cryochemistry bath sedimentation to be prepared from.
The method comprises the following steps:
1) substrate is cleaned
The each ultrasonic cleaning of deionized water 15 minutes of ethanol, acetone are put in the substrate of FTO electro-conductive glass successively and being added with washing agent is to remove dust and the grease of substrate surface, put into deionized water for ultrasonic again and clean 15 minutes, wash away the washing agent containing dirt and some inorganic pollutions, and then within ultrasonic 15 minutes, carry out rinsing with deionized water, finally dry up for subsequent use with nitrogen.
2) preparation of chemical bath deposition solution
By 4.74g(12.5mmol) lead acetate, 2g(50mmol) NaOH, 1.52g(20mmol) thiocarbamide and 1.49g(10mmol) triethanolamine is dissolved in 400ml deionized water, forms solution A after stirring.By 0.64g(3.75mmol) copper chloride and 1.19g(8mmol) triethanolamine is dissolved in 100ml deionized water, forms solution B after stirring.Then under agitation solution A is slowly joined in solution B, continue stirring and form chemical bath deposition solution after 10 minutes.
3) at FTO glass basic surface deposition Pb
xcu
1-xs is to electrode
The FTO electro-conductive glass substrate cleaned up is fixed on fixture, then substrate is dipped vertically in deposit solution, after the beaker filling solution being sealed with aluminium foil, be placed on magnetic stirring apparatus and at room temperature carry out deposition reaction, after deposition a period of time, form one deck khaki or pewter Pb at FTO glass basic surface
xcu
1-xs film, the longer color of sedimentation time is darker.Reaction terminates rear taking-up electrode, clean with deionized water rinsing, and for subsequent use by oven for drying.
Further, Pb in the deposit solution described in step (2)
2+source can be lead acetate or plumbi nitras, Cu
2+source can be copper chloride or copper acetate, wherein Pb
2+, Cu
2+and S
2-mol ratio be 10:3:16.
Further, the deposit solution described in step (2) is strong basicity, and pH value is about 13.
Further, the sedimentation time described in step (3) is 2 ~ 15 hours, the Pb of formation
xcu
1-xthe thickness of S Catalytic Layer is 150 ~ 700nm.
Compared with prior art, the invention provides a kind of for replacing conventional P t to the efficient Pb of electrode
xcu
1-xs is to electrode material and conveniently preparation method, and advantage of the present invention is:
1) with Pt to compared with electrode, Pb
xcu
1-xs has higher catalytic activity to electrode pair many sulphur electrolyte, can promote the electric transmission to electrode/electrolyte interface, thus significantly improves the photoelectric conversion efficiency of battery, significantly can reduce the production cost of battery simultaneously.
2) with PbS or CuS prepared by tinsel to compared with electrode, Pb prepared by the present invention
xcu
1-xs to electrode and substrate adhesion good, enhance the stability to electrode, and be convenient to the encapsulation of battery.
3) Pb
xcu
1-xs is at room temperature prepared from by solwution method electrode, and technique is simple, with low cost, the method be applicable to prepare on a large scale based on flexible conducting substrate to electrode.
accompanying drawing illustrates:
For making those skilled in the art understand technical scheme of the present invention better, below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.These embodiments only for illustration of object of the present invention, its scope do not limited the present invention in any way.
Fig. 1 (a) ~ (d) be respectively method of the present invention with FTO substrate, deposition 2 hours, 7 hours and 15 hours preparation Pb
xcu
1-xs electrode SEM schemes,
Fig. 2 is the Pb of method of the present invention in deposition preparation in 7 hours
xcu
1-xs electrode section SEM schemes,
Fig. 3 is that method of the present invention is at the Pb prepared for 7 hours with FTO substrate and deposition
xcu
1-xs electrode XRD schemes,
Fig. 4 is the Pb that method of the present invention is prepared with different sedimentation time
xcu
1-xs to the QDSSC current-voltage curve figure of electrode assembling,
Fig. 5 is that method of the present invention is with the QDSSC current-voltage curve figure of Pt to electrode assembling.
Embodiment 1
(1) Pb is prepared
xcu
1-xs is to electrode
1) substrate is cleaned
The each ultrasonic cleaning of deionized water 15 minutes of ethanol, acetone are put in the substrate of FTO electro-conductive glass successively and being added with washing agent is to remove dust and the grease of substrate surface, put into deionized water for ultrasonic again and clean 15 minutes, wash away the washing agent containing dirt and some inorganic pollutions, then within ultrasonic 15 minutes, carry out rinsing with deionized water, finally dry up with nitrogen for subsequent use.
2) preparation of chemical bath deposition solution
By 4.74g(12.5mmol) lead acetate, 2g(50mmol) NaOH, 1.52g(20mmol) thiocarbamide and 1.49g(10mmol) triethanolamine is dissolved in 400ml deionized water, forms solution A after stirring.By 0.64g(3.75mmol) copper chloride and 1.19g(8mmol) triethanolamine is dissolved in 100ml deionized water, forms solution B after stirring.Then under agitation solution A is slowly joined in solution B, continue stirring and form chemical bath deposition solution after 10 minutes, Pb
2+, Cu
2+and S
2-mol ratio be 10:3:16.
3) at electro-conductive glass substrate surface deposition Pb
xcu
1-xs is to electrode
The FTO electro-conductive glass substrate cleaned up is fixed on fixture, then substrate is dipped vertically in deposit solution, after the beaker filling solution being sealed with aluminium foil, be placed on magnetic stirring apparatus and at room temperature carry out deposition reaction, deposit and take out FTO substrate after 2 hours, clean with deionized water rinsing, and for subsequent use by oven for drying, its thickness of scanning electron microscope test is used to be 173nm, this electrode called after Pb
xcu
1-xs-2.
(2) the porous TiO of CdSe quantum dot sensitization is prepared
2light anode (TiO
2/ CdSe)
By silk screen print method by Dyesol-18NRTTiO
2slurry is coated on FTO electro-conductive glass, and then anneal 30 minutes in the Muffle furnace of 500 DEG C, forming thickness after being down to room temperature is 10 μm, and area is 5 × 5mm
2porous TiO
2electrode.Adopt electrochemical deposition method (X.Song, etal., ElectrochimicaActa, 2013,108,449) at porous TiO subsequently
2surface deposition CdSe quantum dot, forms TiO
2/ CdSe electrode.
(3) assembling quantum dot sensitization solar battery testing
By the TiO prepared
2/ CdSe light anode is placed on table top, and the heat-sealing film cut " back-shaped " framework (60 μm) is overlayed above-mentioned electrode surrounding, then in heat-sealing film surface cover to electrode, make to be packaged together to electrode and light anode with heat sealing machine heating, then by pouring into many sulphur electrolyte (1mol/LNa to the aperture that electrode is accomplished fluently in advance
2the aqueous solution of S and 1mol/LS powder), the preparation of quantum dot sensitization solar battery then can be completed with heat-sealing film sealed aperture.The battery assembled is at 100mW/cm
2(AM1.5) measuring current-voltage curve under simulated solar irradiation.
Embodiment 2
(1) Pb is prepared
xcu
1-xs is to electrode
1) substrate is cleaned
With embodiment 1.
2) preparation of chemical bath deposition solution
With embodiment 1.
3) at electro-conductive glass substrate surface deposition Pb
xcu
1-xs is to electrode
The FTO electro-conductive glass substrate cleaned up is fixed on special fixture, then substrate is dipped vertically in deposit solution, after the beaker filling solution being sealed with aluminium foil, be placed on magnetic stirring apparatus and at room temperature carry out deposition reaction, deposit and take out FTO substrate after 4 hours, clean with deionized water rinsing, and for subsequent use by oven for drying, its thickness of scanning electron microscope test is used to be 324nm, this electrode called after Pb
xcu
1-xs-4.
(2) the porous TiO of CdSe quantum dot sensitization is prepared
2light anode (TiO
2/ CdSe)
With embodiment 1.
(3) assembling quantum dot sensitization solar battery testing
With embodiment 1.
Embodiment 3
(1) Pb is prepared
xcu
1-xs is to electrode
1) substrate is cleaned
With embodiment 1.
2) preparation of chemical bath deposition solution
With embodiment 1.
3) at electro-conductive glass substrate surface deposition Pb
xcu
1-xs is to electrode
The FTO electro-conductive glass substrate cleaned up is fixed on special fixture, then substrate is dipped vertically in deposit solution, after the beaker filling solution being sealed with aluminium foil, be placed on magnetic stirring apparatus and at room temperature carry out deposition reaction, deposit and take out FTO substrate after 7 hours, clean with deionized water rinsing, and for subsequent use by oven for drying, its thickness of scanning electron microscope test is used to be 582nm, this electrode called after Pb
xcu
1-xs-7.
(2) the porous TiO of CdSe quantum dot sensitization is prepared
2light anode (TiO
2/ CdSe)
With embodiment 1.
(3) assembling quantum dot sensitization solar battery testing
With embodiment 1.
Embodiment 4
(1) Pb is prepared
xcu
1-xs is to electrode
1) substrate is cleaned
With embodiment 1.
2) preparation of chemical bath deposition solution
With embodiment 1.
3) at electro-conductive glass substrate surface deposition Pb
xcu
1-xs is to electrode
The FTO electro-conductive glass substrate cleaned up is fixed on special fixture, then substrate is dipped vertically in deposit solution, after the beaker filling solution being sealed with aluminium foil, be placed on magnetic stirring apparatus and at room temperature carry out deposition reaction, deposit and take out FTO substrate after 10 hours, clean with deionized water rinsing, and for subsequent use by oven for drying, its thickness of scanning electron microscope test is used to be 638nm, this electrode called after Pb
xcu
1-xs-10.
(2) the porous TiO of CdSe quantum dot sensitization is prepared
2light anode (TiO
2/ CdSe)
With embodiment 1.
(3) assembling quantum dot sensitization solar battery testing
With embodiment 1.
Embodiment 5
(1) Pb is prepared
xcu
1-xs is to electrode
1) substrate is cleaned
With embodiment 1.
2) preparation of chemical bath deposition solution
With embodiment 1.
3) at electro-conductive glass substrate surface deposition Pb
xcu
1-xs is to electrode
The FTO electro-conductive glass substrate cleaned up is fixed on special fixture, then substrate is dipped vertically in deposit solution, after the beaker filling solution being sealed with aluminium foil, be placed on magnetic stirring apparatus and at room temperature carry out deposition reaction, deposit and take out FTO substrate after 15 hours, clean with deionized water rinsing, and for subsequent use by oven for drying, its thickness of scanning electron microscope test is used to be 672nm, this electrode called after Pb
xcu
1-xs-15.
(2) the porous TiO of CdSe quantum dot sensitization is prepared
2light anode (TiO
2/ CdSe)
With embodiment 1.
(3) assembling quantum dot sensitization solar battery testing
With embodiment 1.
Fig. 1 (a) is the surperficial SEM figure of FTO electro-conductive glass substrate, can see the coarse injustice of FTO conductive glass surface, SnO
2particle size is uneven, and corner angle are clearly demarcated, in irregular fish scale-shaped.Fig. 1 (b) ~ (d) be respectively deposition 2 hours, 7 hours and 15 hours preparation Pb
xcu
1-xs electrode surface SEM schemes, as we can see from the figure when deposited between be 2 constantly little, SnO
2the corner angle of particle become more mellow and fuller, imply some nano particles of its surface deposition, but the surface appearance feature of FTO is still visible, illustrate that the coverage rate of nano particle to FTO of deposition is lower, these exposed FTO substrates do not have catalytic activity to many sulphur electrolyte, have adverse effect after being assembled into device to battery performance.After extending to 7 hours when deposited, the nano particle of FTO surface deposition one deck even compact can be seen significantly, and the shape characteristic of FTO fades away, illustrate that nano particle improves the coverage rate of FTO.Continue when deposited to extend to 15 hours, nanoparticle size becomes large, and the film of deposition is more and more thicker.And be engaged in matter sample and can see that sample surfaces is smoothly fine and close, do not have crackle to occur, show that the film obtained has preferable quality.
Fig. 2 is the Pb of deposition preparation in 7 hours
xcu
1-xs electrode section SEM schemes, Pb as we can see from the figure
xcu
1-xthe Thickness Ratio of S film is comparatively even, is about 582nm.
Fig. 3 is the Pb of deposition preparation in 7 hours
xcu
1-xs electrode XRD schemes, as can be seen from the figure, except substrate SnO
2diffraction maximum outside, there is again several new diffraction maximum (with mark), contrast with standard diagram (JCPDSNo.05-0592) and find, be positioned at 2 θ=26.02 °, 30.16 °, 43.12 °, the diffraction maximum of 71.04 ° and 84.26 ° corresponds respectively to (111) of Emission in Cubic rock salt structure PbS, (200), (220), and (511) crystal face (420), illustrate in film containing this component of PbS, and be positioned at 2 θ=27.50 °, the diffraction maximum (with mark) of 31.34 ° and 47.46 °, with hexagonal crystal system CuS(JCPDSNo.06-0464) (101), (103) and (110) crystal face corresponding, illustrate in film containing this component of CuS, thus prove that prepare is Pb
xcu
1-xs film.
Fig. 4 is the Pb prepared by different sedimentation time
xcu
1-xs is to the current-voltage curve of the quantum dot sensitized battery of electrode assembling, and table 1 is the photoelectric properties parameter obtained from figure.Can see based on Pb from table
xcu
1-xthe cell photoelectric conversion efficiency of S-2 to electrode is very low, only has 0.95%, and this is the Pb due to FTO substrate surface deposition
xcu
1-xvery little, the exposed FTO of major part does not have catalytic activity to many sulphur electrolyte to S catalyst amounts, too large to electrode/electrolyte interface resistance, has had a strong impact on the performance of battery.Extend to 7 hours when deposited, the PbS catalyst of FTO surface deposition increases, and improves further, make Pb to the catalytic performance of electrode
xcu
1-xthe cell photoelectric conversion efficiency of S-7 structure reaches 2.39%.When continuing when deposited to increase, Pb
xcu
1-xthe thickness of S increases further, and the interior resistive making paired electrode is large, thus makes to reduce the catalytic performance of electrode, and the photovoltaic parameter of battery declines.
Each ZnO/PbS of table 1 is to the QDSSC photoelectric properties parameter of electrode assembling
Embodiment 6
(1) Pt is prepared to electrode (comparison electrode)
1) substrate is cleaned
With embodiment 1.
2) magnetron sputtering method is adopted to deposit at FTO substrate surface the Pt Catalytic Layer that a layer thickness is about 100nm.
(2) the porous TiO of CdSe quantum dot sensitization is prepared
2light anode (TiO
2/ CdSe)
With embodiment 1.
(3) assembling quantum dot sensitization solar battery testing
With embodiment 1.
Fig. 5 is the current-voltage curve of Pt to the QDSSC of electrode assembling, and the cell photoelectric conversion efficiency of Pt assembling is as we can see from the figure 1.22%, lower than Pb
xcu
1-xthe photoelectric conversion efficiency of S-7 electrode 2.39%, this causes because the catalytic activity of Pt to many sulphur electrolyte is more weak.
Claims (5)
1. one kind for quantum dot sensitized solar cell to electrode and preparation method thereof, it is characterized in that: be grow at FTO electro-conductive glass substrate surface the Catalytic Layer that one deck is made up of PbS and CuS to the structure of electrode, this Catalytic Layer adopts cryochemistry bath sedimentation to be prepared from.
2. according to claim 1 a kind of for quantum dot sensitized solar cell to electrode and preparation method thereof, it is characterized in that comprising the following steps:
1) substrate is cleaned
The each ultrasonic cleaning of deionized water 15 minutes of ethanol, acetone are put in the substrate of FTO electro-conductive glass successively and being added with washing agent is to remove dust and the grease of substrate surface, put into deionized water for ultrasonic again and clean 15 minutes, wash away the washing agent containing dirt and some inorganic pollutions, and then within ultrasonic 15 minutes, carry out rinsing with deionized water, finally dry up for subsequent use with nitrogen;
2) preparation of chemical bath deposition solution
By 4.74g(12.5mmol) lead acetate, 2g(50mmol) NaOH, 1.52g(20mmol) thiocarbamide and 1.49g(10mmol) triethanolamine is dissolved in 400ml deionized water, forms solution A after stirring; By 0.64g(3.75mmol) copper chloride and 1.19g(8mmol) triethanolamine is dissolved in 100ml deionized water, forms solution B after stirring; Then under agitation solution A is slowly joined in solution B, continue stirring and form chemical bath deposition solution after 10 minutes;
3) at FTO glass basic surface deposition Pb
xcu
1-xs is to electrode
The FTO electro-conductive glass substrate cleaned up is fixed on fixture, then substrate is dipped vertically in deposit solution, after the beaker filling solution being sealed with aluminium foil, be placed on magnetic stirring apparatus and at room temperature carry out deposition reaction, after deposition a period of time, form one deck khaki or pewter Pb at FTO glass basic surface
xcu
1-xs film, the longer color of sedimentation time is darker; Reaction terminates rear taking-up electrode, clean with deionized water rinsing, and for subsequent use by oven for drying.
3. according to claim 2 a kind of for quantum dot sensitized solar cell to electrode and preparation method thereof, it is characterized in that: Pb in the deposit solution described in step (2)
2+source can be lead acetate or plumbi nitras, Cu
2+source can be copper chloride or copper acetate, wherein Pb
2+, Cu
2+and S
2-mol ratio be 10:3:16.
4. according to claim 2 a kind of for quantum dot sensitized solar cell to electrode and preparation method thereof, it is characterized in that: the deposit solution described in step (2) is strong basicity, and pH value is about 13.
5. according to claim 2 a kind of for quantum dot sensitized solar cell to electrode and preparation method thereof, it is characterized in that: the sedimentation time described in step (3) is 2 ~ 15 hours, the Pb of formation
xcu
1-xthe thickness of S Catalytic Layer is 150 ~ 700nm.
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| CN106129142A (en) * | 2016-06-24 | 2016-11-16 | 中原工学院 | A kind of preparation method of vulcanized lead quantum dot |
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| CN107315215B (en) * | 2017-06-15 | 2020-12-08 | 中国科学院合肥物质科学研究院 | Lead sulfide film with wide absorption spectrum and preparation method thereof |
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